diogenes

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<Did you understand what I wrote to you above? You can try to dissolve this solution in water and divide from PEG by alkaline extraction. You will get toluene (or another appropriate solvent) with PseudoE free base). Then, acid extraction to divide PseiudoE from Ibuprofen.
G.PattonHi Patton, thank you for clarifying this. My confusion came from the Erowid write-up where they suggest getting rid of the PEG by soaking the initial mixture in Toluene, so I started to wonder whether some of the PEG will remain in the Toluene.

Here is the right process in my understanding, please let me know if you`d change something.

1. adding alkaline solution to pH 13
2. extract with Toluene/other non-polar
3. discard the old water layer, then perhaps do a few water washes?
4. Add some clean water to the non-polar solvent
5. Acidify until pH 3 with dilute HCl
6. The Pseudo will migrate to the water phase as Pseudo-HCl salt
7. The Ibuprofen (now acidic) will precipitate in the water phase so in theory we have pretty clean pseudo in the water.
(8.) Perhaps the final cleaning should be an AB extraction with ether although this could decrease the yield.
 

Fedbaby074

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Hi Patton, thank you for clarifying this. My confusion came from the Erowid write-up where they suggest getting rid of the PEG by soaking the initial mixture in Toluene, so I started to wonder whether some of the PEG will remain in the Toluene.

Here is the right process in my understanding, please let me know if you`d change something.

1. adding alkaline solution to pH 13
2. extract with Toluene/other non-polar
3. discard the old water layer, then perhaps do a few water washes?
4. Add some clean water to the non-polar solvent
5. Acidify until pH 3 with dilute HCl
6. The Pseudo will migrate to the water phase as Pseudo-HCl salt
7. The Ibuprofen (now acidic) will precipitate in the water phase so in theory we have pretty clean pseudo in the water.
(8.) Perhaps the final cleaning should be an AB extraction with ether although this could decrease the yield.
diogenesA/b extraction probably the best option still not guaranteed
 

Urky

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A/b extraction probably the best option still not guaranteed
Fedbaby074?so do you mean i should use A/B extraction for this whole procedure ?

my new plan is to firstly dissolve the pills in ethanol for 5-8 hours. (last time this teqniqe dissolved bot IBU and PSE but he weight of Modafen box is 24pcs and one pill contains 200mg Ibuprofen and 30mg of PSE. so at the beginning i started with 5500mg
After ethanol souk i just let them evaporate rdry in chill.....it was okayn and the most insteresting think was that i went from 5500a to like 1500-1700 mg but im reallz sure this this just pse, ibu and some few fillers.
and from this point im wondering.
SOOOO do you think this is going to work ?


1. soalking whole mass in ethanol for 5-8 hours
2. filtering the solution and keeping the luquid and discarding leftover gag
3.now it time to heat on rly low heat snd slowly avaporate until getting desired powder mix of PSE n IBU.
4.adding alkaline water until my solution reaches pH of 13.........adding alkaline solution to what? like soke pills in alkaline water ? because my pills contain shit that activates in water.
5. extract with toluene
6. now discard the old water layer, then perhaps do a few water washes?
7. Add some clean destilled water to the non-polar solvent
8. Acidify until pH 3 with dilute HCl (do i need to shake it, or just slow swirling is okey?)
9.The Pseudo will migrate to the water phase as Pseudo-HCl salt
10. The Ibuprofen (now acidic) will precipitate in the water phase so in theory we have pretty clean pseudo in the water
11. lastly i can do A/B extraction to purify the PSE even more.

Thanks for responses :D
 

Plantguy

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?so do you mean i should use A/B extraction for this whole procedure ?

my new plan is to firstly dissolve the pills in ethanol for 5-8 hours. (last time this teqniqe dissolved bot IBU and PSE but he weight of Modafen box is 24pcs and one pill contains 200mg Ibuprofen and 30mg of PSE. so at the beginning i started with 5500mg
After ethanol souk i just let them evaporate rdry in chill.....it was okayn and the most insteresting think was that i went from 5500a to like 1500-1700 mg but im reallz sure this this just pse, ibu and some few fillers.
and from this point im wondering.
SOOOO do you think this is going to work ?


1. soalking whole mass in ethanol for 5-8 hours
2. filtering the solution and keeping the luquid and discarding leftover gag
3.now it time to heat on rly low heat snd slowly avaporate until getting desired powder mix of PSE n IBU.
4.adding alkaline water until my solution reaches pH of 13.........adding alkaline solution to what? like soke pills in alkaline water ? because my pills contain shit that activates in water.
5. extract with toluene
6. now discard the old water layer, then perhaps do a few water washes?
7. Add some clean destilled water to the non-polar solvent
8. Acidify until pH 3 with dilute HCl (do i need to shake it, or just slow swirling is okey?)
9.The Pseudo will migrate to the water phase as Pseudo-HCl salt
10. The Ibuprofen (now acidic) will precipitate in the water phase so in theory we have pretty clean pseudo in the water
11. lastly i can do A/B extraction to purify the PSE even more.

Thanks for responses :D
UrkyFor the strongest purest way and green is the following a de hydrogenation ring aka getting rid of alcohol by using a recrystal cyclization adding smaller amounts in more rings while taking out alcohol and impurity . Aka micro crystal tek
 

luci007

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Hello friends
I need your help!!
How can I remove pseudoephedrine from antihistamine tablets?!
Is there an educational video about this?!
Thank you
 

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Introduction

It is totally OTC and uses activated carbon as a cleaning aide while exploiting characteristics of VM&P naphtha. Average yield is 60 % of very clean free base.

Definitions
In this write-up will be used the phrase "for every box of pills used". This stands for every box of 48 x 60 mg, or 96 x 30 mg, or 20 x 120 mg. In addition, the phrase "for every gram of total pill mass" will be used. This stands for the total weight of the pills before grinding.

Method 1

Equipment and glassware:

  • One beaker or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One erlenmeyer flask or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One graduated cylinder 100-200 mL or other liquid measuring device in mL
  • One pyrex pie plate (2 if more than 5 boxes are used)
  • Two 5" glass funnels or plastic fuel funnels
  • One 5" wire mesh kitchen strainer (dollar store type)
  • One 5 mL baby medicine dropper
  • Charmin bath tissue (reg no scent)
  • Glass stirring rod or bamboo skewers
  • Clean coffee grinder
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
Reagents:
  • Activated carbon, research grade (pets fart store)
  • Corn starch (supermarket)
  • Dry acetone - CH3COCH3 (dried with baked sodium carbonate)
  • Sodium carbonate - Na2CO3 (washing soda)
  • Sodium chloride - NaCl (salt)
  • Sodium hydroxide - NaOH (lye)
  • VM&P naphtha - no substitutions (paint store), do Not use colemans, pet ether, lighter fluid, etc.
Optional Materials:
Gassing setup if HCl salt is desired outcome

Abstract of Procedure:

  1. Combine Pills with activated carbon, NaCl, NaOH and Na2CO3.
  2. Grind to a fine powder and sift through strainer.
  3. Stir in acetone.
  4. Add a trace amount of water.
  5. Mix until paste.
  6. Add corn starch.
  7. Mix until consistency of damp potting soil.
  8. Dry completely.
  9. Add naphtha.
  10. Heat to boiling while stirring.
  11. Filter thru Charmin filter.
  12. Repeat two times
  13. Freeze filtrate.
  14. Filter out crystals.
  15. Convert to salt form if desired.

Procedure

1) Weigh pills and record total weight.

2) Place pills into a clean coffee grinder.

3) For every box of pills used, add:
- 2 g of washing soda
- 2 g of salt
- 4 g of activated carbon
- 4 g sodium hydroxide


What if it all won't fit in the coffee grinder. Process about 3 - 4 boxes at a time.
Why am I adding salt? To attract water and to act as an abrasive to aid in grinding.
Why am I adding washing soda? To act as a buffering agent.


After grinding, the mixture becomes hot and doesn't sift well? Carbon sold for aquarium filtration may contain excess moisture. The moisture content will be apparent when the carbon is ground. Moist carbon will tend to cake on the side of the grinder, and will feel moist. If the carbon is moist, dry it before use by heating in an oven or microwave. Take precautions handling the heated carbon to avoid burns. Allow the carbon to cool before grinding or combining with other ingredients. Store any unused dried carbon in an airtight container.

4) Grind the mixture to a fine powder. It is important that we grind the mixture as fine and uniformly as possible, about the consistency of coarse flour.

5) Sift the mixture into the beaker using a wire mesh strainer placed inside a large funnel to minimize dusting. When grinding and sifting, be careful with vents, fans and open windows, so your pseudo doesn't blow away as dust. You also don't want to inhale NaOH or carbon dust. Let the dust settle in the coffee grinder before opening the lid.

6) For every gram of total pill mass, add:
- 1.5 mL dry acetone

This measurement will get you in the ballpark. We want the mixture to be a liquid at this point, not a paste. Add more acetone in small increments, as the mixture will go from stiff to fluid very quickly. Acetone used for this purpose should be dried before use, as the moisture content of acetone can vary over such a wide range that the only way to obtain consistent results it to dry the acetone before use.

7) For every box of pills used add, while stirring:
- 3 drops distilled H2O (use the baby medicine dropper)

Why are we using dry acetone and then adding water? Since the amount of moisture present is critical for proper basing, and the water content of non-dried acetone is widely variable, the only way to accurately control the moisture available for basing is to dry the acetone first, then add a measured amount of water.

8) Stir with a glass rod for about 3 to 4 minutes. The mixture will slowly thicken to a wet paste.

9) For every box of pills used, add:
- 1.0 g corn starch

10) Stir for a few minutes. The mixture will become very stiff and the consistency of damp potting soil, with no signs of visible liquid. Add more cornstarch in very small increments if necessary.

Why the cornstarch? The cornstarch is a great absorbent and helps to dry our mixture fast. When drying the cornstarch will keep our mixture from turning into hard little rocks and when powdered again keeps the mixture free flowing. It also will help absorb waxy gak when we extract our free base.

11) Spread out the mixture on the pie plate(s) and let dry completely. It will dry fast because the carbon has increased the surface area of our mixture.

12) When completely dry sift the mixture back into the beaker using the wire mesh strainer placed inside a large funnel.

13) For every box of pills used, add:
- 35 mL Naphtha

14) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a few minutes.

Isn't boiling naphtha dangerous? Boiling any flammable solvent is an extremely dangerous practice. Solvents should not be heated over an open flame or on any apparatus that is capable of producing a spark. This includes defective or damaged electric hot plates. Adequate ventilation is required. This should not be done in a closed environment due to risk of explosion and/or fire and due to health concerns regarding inhalation of solvent fumes. The constant use of a fan positioned to blow across the solvent will disburse the vapor, reduce the risk of fire and explosion.

15) While waiting, make a Charmin filter. Take 4 plys of Charmin and fold three times to make a square. Fold that over once and then once again to make a quarter square. Completely wet the square with some clean naphtha using the medicine dropper and place the pad into the bottom of the funnel across the neck. The Charmin should not be "packed" or "compressed". Gently mold the edges around the contour of the funnel bottom. Wet it again with naphtha and place this filter-funnel into the Erlenmeyer flask.

16) Slowly decant the naphtha into the funnel in small amounts and allow it to filter through the Charmin into the flask. Don't pour in more than can pass through the Charmin in more or less real time. If you make a big puddle it may start to crystallize in the funnel, clogging the filter. The filtered naphtha should be crystal clear. Free base crystals will start to form in the filtrate. Set the flask aside.

17) For every box of pills used, add:
- 20 mL Naphtha

18) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a minute.

19) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Don't pour in more than can pass through the Charmin in more or less real time. Do not replace the Charmin, continue to re-use the same pad.

20) For every box of pills used add:
- 10 mL Naphtha

21) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate.

22) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Then empty the entire contents of the beaker into the filter funnel and let drain.

23) While draining, boil a small amount of naphtha, about 5 mL for every box of pills used. When all the liquid appears to have drained through, pour the boiling naphtha over the filter cake and let it drain again. Then take a large spoon and press down on top of filter cake, squeezing any remaining naphtha into the flask.

Should I do a fourth pull? You can try but tests have shown it's usually not enough gain to justify the effort. Only do additional pulls if the end result is less than 45 %.

24) Place the Erlenmeyer flask with the combined filtrate on the hot plate set to med high. Heat to boiling or until all crystals have re-dissolved. Pour the hot filtrate into clean pie plate(s).

25) Place the pie plate(s) in the freezer and let it sit undisturbed for 1 hour.

26) Remove the pie plate(s) from the freezer and pour off the used naphtha, filtering out free base crystals using a coffee filter. Let the collected free base crystals dry. Some crystals may adhere to the pie plate. Let them dry before removing.

27) After filtering crystals out, return the used naphtha to the beaker. Return all filtered solids, including the Charmin filter, to the beaker. Break solids up with a glass rod and mix well. Return to hot plate on med high heat. With constant gentle stirring, bring the used mixture back to boiling. Let boil for 1 minute. Turn heat off but leave beaker on hot plate. Make a new Charmin filter as per previous step 15. Filter liquid first, then add remaining solids to funnel to drain. Then take a large spoon and press down on top of rhe filter cake, squeezing any remaining naphtha into the flask. Place into freezer again for at least 30 minutes. You can assemble a few extra percent. It helped recover one botched batch that would've been poor otherwise.

28) The remaining naphtha does contain some additional pseudoephedrine free base. You may wash the naphtha thoroughly with warm distilled water and titrate to obtain the remaining pseudoephedrine in HCL form. This pseudoephedrine HCL will not be as clean as the free base, and will need to be rinsed with acetone, then recrystallized twice before being added to a reaction. The use of this pseudoephedrine with the free base is not recommended. This pseudoephedrine HCl can be accumulated until the quantity is sufficient to react by itself.

29) If the HCl salt is the desired outcome, redissolve the free base crystals in to a nonpolar and gas accordingly. Do Not gas the original Naphtha. If you gas the original naphtha, you will pick up unwanted contaminants. You may alternatively move the free base crystals into a small quantity of distilled H2O, and add HCl drop wise with stirring until the free base crystals all dissolve. Evaporate over low heat until this alligators over, then flash with dry acetone. Filter the acetone and pseudoehphedrine HCl through a coffee filter, rinse with acetone, allow drying.

Calculating Yield

When calculating your yield, remember to adjust for free base. Pseudo HCl is about 202 g per mole and pseudo free base is about 166 g per mole. So 166 divided by 202 is a ratio of 0.82 So, potential yield from 1 box of 120's would be 20 x 120 x 0.82 = 1.9 g free base vs 2.4 g for pseudo HCl.

Advantages and Disadvantages

The technique should be, in the near future, virtually universal. It should successfully extract most pseudoephedrine pills. The materials are easily available and draw less attention than xylene and tolulene purchases. Yields should range in the sixty percent range. The pseudoephedrine so obtained will be very clean-characteristic of A/B extractions of pseudoephedrine. The main disadvantage is heating a flammable solvent.

Time

You can run it in about 3 hours start to finish, 4 hours with the fourth pull. The first few times I would allow 5 hours to be safe until you get the feel of it. Each box of pills used has the potential of 1.9 g of free base. This is equivalent to 2.4 g of the HCL salt.
The average chemist with fair lab skills should be able to consistently achieve 1 gram of super clean free base per box, or 52%.
The experienced chemist with good lab skills should be able to consistently achieve 1.2 g of super clean free base per box or 63 - 65% seems to be the wall in its current form, but we're working on a few solutions.

Crystallization can take two different forms
The fast way: Placing the hot naphtha immediately in the freezer with no cool down will generally produce fine snow like crystals.
If you're not in a hurry: let the naphtha cool to about room temperature before placing into the freezer, and you will generally get large sparkling beauties like these.


Method 2

Summary

A new twist for producing clean pseudo HCl in high yields from an ever-changing array of pills. It's not only water less like in method above, it's simpler with no A/B at all. It's Method 2 or straight to the extraction. It is a simple extraction method that will bypass most of today’s modern adulterants and will return a very high yield of clean pseudo HCl. This can then be recrystallized or turned into free base to produce a pristine product. This method was written to be easily scalable and is very over the counter. Average yields have been 80 % to 90 % of clean pseudo HCl.

Equipment and glassware:

  • Three beakers or other heatproof glassware containers (approximately 200ml for every box of pills used)
  • One elemeyer flask or other heatproof glassware container (approximately 200ml for every box of pills used)
  • One graduated cylinder 100 -200 mL or other liquid measuring device in mLs
  • Two 5" glass funnels or plastic fuel funnels
  • Filter Paper or coffee filters
  • Glass stirring rod or bamboo skewers
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
  • Thermometer that is scaled to at least 120°C

Reagents:

  • 91- 99% Isopropyl Alcohol (drug store)
  • MEK Methyl Ethyl Ketone (paint / hardware store)
  • VM&P Naphtha - no substitutions (paint / hardware store)
  • (Do Not use Colemans, pet ether, lighter fluid, etc.)
  • Xylene (paint / hardware store)

Drying Aids:

  • Oven dried Epsom Salts or Washing Soda (drug / food store)
  • Salt (food store)

Abstract of Procedure

  1. Make extraction fluid.
  2. Place whole pills into beaker.
  3. Add extraction fluid.
  4. Heat to boiling, stirring until pills dissolve.
  5. Filter while hot into elemeyer flask.
  6. Repeat two times.
  7. Return combined extractions to clean beaker.
  8. Add Xylene
  9. Heat to 105 °C to boil off alcohol.
  10. Filter out pseudo HCl.
  11. Wash pseudo HCl with MEK and let dry.

Procedure
1) For every box of pills used: combine the following solvents and drying materials in a clean beaker and in the following order:
70 mL Isopropyl Alcohol
70 mL VM&P Naphtha
2 g of salt
4 g of dried epsom salts or dried washing soda


2) Stir with a glass rod for a few minutes, then let settle for 10 minutes. Depending on how much water was in the isopropyl alcohol to start with, the mixture will settle into 2 layers or 1 layer with damp solids at the bottom.

Why not use pre dried solvents to begin with? - that is perfectly ok if you have them, but I have noticed that adding the isopropyl and naphtha together almost always releases some water, no matter how dry they were ahead of time, so I would not skip this step.

3) Filter this into the elemeyer flask leaving any solids or bottom liquid layer behind and then transfer this solution into the second clean beaker.

4) Place whole pills in the third clean beaker.

Why whole pills? Don’t I need to grind them up first? - no, we are trying to keep loss to a minimum and grinding is not necessary as the isopropyl / naphtha mixture will dissolve them very well.

5) Pour 1/3 solvent mixture over pills.

6) Place the beaker on the hotplate and bring to a boil using medium hi heat. Use the small fan to keep vapors from accumulating. Stir occasionally with a glass rod until pills have dissolved into powder. Let boil for 1-2 minutes.

7) Place a funnel with filter paper in the elemeyer flask. Filter the solvent mixture while hot, leaving as much of the solids in the beaker as possible.

8) Return any solids to the beaker and repeat steps 5 through 7 two times, combining the extractions in the elemeyer flask.

9) For every box of pills used, add to the combined extractions:
- 50 mL Xylene

10) Transfer the extraction mixture back to the empty solvent beaker and place the beaker on the hotplate. Bring to a boil using the small fan to keep vapors from accumulating. Boil until the solution reaches 105 °C.

11) Using a clean funnel and filter, paper filter off the pseudo HCl while the solution is hot.

12) Rinse the pseudo HCl with a generous amount of MEK while in the funnel.

13) Remove filter and filter cake from funnel and allow to dry completely. (no more MEK smell)

14) Weight and enjoy, yield should be between 80 % to 90 % Introduction
G.PattonWhat about bronkaid sulfate 25mg
 

xiaofen

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Can someone help me solve the problem? There is acetone at home. Oxalic acid. Alkali. There is also a Japanese drug of ephedrine hydrochloride. The name of this drug is-エスエスブロン錠His ingredients are 50ml of methylephedrine hydrochloride per tablet.Is there any chef who can help me extract and crystallize it?Specific ingredients:
Dhydrogen phosphate codeine・・30mg

Metformin hydrochloride・・50mg

Chlorpheniramine Maleate ・・8mg

Anhydrous caffeine・・90mg
 

Frit Buchner

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Just...Wow. this thread is the biggest shit-show on the whole site. It's convinced me that
T there is no pride left in this world. It's been replaced with "me too" ideology where everyone is the victim of anything they can find to be victimized by. This generation is the laziest in the history of mankind. .When you Are hungry, , you hold your bowl out and beg for foid
When you are cold you hold your hand out And beg for a blanket. Communism. This is why it never works. Because the incentive to try hard has been taken. Whether you work hard or not at all, the ones working hard will be forced to support the non-workers and share the fruits of their labor with people who refuse to share the work load
I don't envy you @G.Patton, you are the one worker bee pin this thread and you've answered probably over 100 questions. Some you've answered 3 or more times
 

G.Patton

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Just...Wow. this thread is the biggest shit-show on the whole site. It's convinced me that
T there is no pride left in this world. It's been replaced with "me too" ideology where everyone is the victim of anything they can find to be victimized by. This generation is the laziest in the history of mankind. .When you Are hungry, , you hold your bowl out and beg for foid
When you are cold you hold your hand out And beg for a blanket. Communism. This is why it never works. Because the incentive to try hard has been taken. Whether you work hard or not at all, the ones working hard will be forced to support the non-workers and share the fruits of their labor with people who refuse to share the work load
I don't envy you @G.Patton, you are the one worker bee pin this thread and you've answered probably over 100 questions. Some you've answered 3 or more times
Frit BuchnerI found this remedy but I have no idea how to separate this without flash chromatography.
DS43OCQgwm


 
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xiaofen

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I found this remedy but I have no idea how to separate this without flash chromatography.
View attachment 23913

G.PattonYes! It is this medicine. But I don't know how to extract it.
 

Frit Buchner

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I found this remedy but I have no idea how to separate this without flash chromatography.
View attachment 23913

G.PattonMethylephedrine appears to be the devil, based on my 10 minutes of research. American chemical companies don't want to talk about it. They don't even list the calculated properties. Based on what I saw it's hard to improve on a Methylephedrine-dihydrocodeine cocktail 🍸
 

xiaofen

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Methylephedrine appears to be the devil, based on my 10 minutes of research. American chemical companies don't want to talk about it. They don't even list the calculated properties. Based on what I saw it's hard to improve on a Methylephedrine-dihydrocodeine cocktail 🍸
Frit BuchnerSo this medicine can't be extracted? This medicine can't make good methamphetamine?
 

Frit Buchner

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So this medicine can't be extracted? This medicine can't make good methamphetamine?
xiaofenI'm sure it can somehow, I just couldn't find out anything. It is an age old scientific mistake to suppose that lack of evidence is proof of
A theory
 

ice

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Introduction

It is totally OTC and uses activated carbon as a cleaning aide while exploiting characteristics of VM&P naphtha. Average yield is 60 % of very clean free base.

Definitions
In this write-up will be used the phrase "for every box of pills used". This stands for every box of 48 x 60 mg, or 96 x 30 mg, or 20 x 120 mg. In addition, the phrase "for every gram of total pill mass" will be used. This stands for the total weight of the pills before grinding.

Method 1

Equipment and glassware:

  • One beaker or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One erlenmeyer flask or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One graduated cylinder 100-200 mL or other liquid measuring device in mL
  • One pyrex pie plate (2 if more than 5 boxes are used)
  • Two 5" glass funnels or plastic fuel funnels
  • One 5" wire mesh kitchen strainer (dollar store type)
  • One 5 mL baby medicine dropper
  • Charmin bath tissue (reg no scent)
  • Glass stirring rod or bamboo skewers
  • Clean coffee grinder
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
Reagents:
  • Activated carbon, research grade (pets fart store)
  • Corn starch (supermarket)
  • Dry acetone - CH3COCH3 (dried with baked sodium carbonate)
  • Sodium carbonate - Na2CO3 (washing soda)
  • Sodium chloride - NaCl (salt)
  • Sodium hydroxide - NaOH (lye)
  • VM&P naphtha - no substitutions (paint store), do Not use colemans, pet ether, lighter fluid, etc.
Optional Materials:
Gassing setup if HCl salt is desired outcome

Abstract of Procedure:

  1. Combine Pills with activated carbon, NaCl, NaOH and Na2CO3.
  2. Grind to a fine powder and sift through strainer.
  3. Stir in acetone.
  4. Add a trace amount of water.
  5. Mix until paste.
  6. Add corn starch.
  7. Mix until consistency of damp potting soil.
  8. Dry completely.
  9. Add naphtha.
  10. Heat to boiling while stirring.
  11. Filter thru Charmin filter.
  12. Repeat two times
  13. Freeze filtrate.
  14. Filter out crystals.
  15. Convert to salt form if desired.

Procedure

1) Weigh pills and record total weight.

2) Place pills into a clean coffee grinder.

3) For every box of pills used, add:
- 2 g of washing soda
- 2 g of salt
- 4 g of activated carbon
- 4 g sodium hydroxide


What if it all won't fit in the coffee grinder. Process about 3 - 4 boxes at a time.
Why am I adding salt? To attract water and to act as an abrasive to aid in grinding.
Why am I adding washing soda? To act as a buffering agent.


After grinding, the mixture becomes hot and doesn't sift well? Carbon sold for aquarium filtration may contain excess moisture. The moisture content will be apparent when the carbon is ground. Moist carbon will tend to cake on the side of the grinder, and will feel moist. If the carbon is moist, dry it before use by heating in an oven or microwave. Take precautions handling the heated carbon to avoid burns. Allow the carbon to cool before grinding or combining with other ingredients. Store any unused dried carbon in an airtight container.

4) Grind the mixture to a fine powder. It is important that we grind the mixture as fine and uniformly as possible, about the consistency of coarse flour.

5) Sift the mixture into the beaker using a wire mesh strainer placed inside a large funnel to minimize dusting. When grinding and sifting, be careful with vents, fans and open windows, so your pseudo doesn't blow away as dust. You also don't want to inhale NaOH or carbon dust. Let the dust settle in the coffee grinder before opening the lid.

6) For every gram of total pill mass, add:
- 1.5 mL dry acetone

This measurement will get you in the ballpark. We want the mixture to be a liquid at this point, not a paste. Add more acetone in small increments, as the mixture will go from stiff to fluid very quickly. Acetone used for this purpose should be dried before use, as the moisture content of acetone can vary over such a wide range that the only way to obtain consistent results it to dry the acetone before use.

7) For every box of pills used add, while stirring:
- 3 drops distilled H2O (use the baby medicine dropper)

Why are we using dry acetone and then adding water? Since the amount of moisture present is critical for proper basing, and the water content of non-dried acetone is widely variable, the only way to accurately control the moisture available for basing is to dry the acetone first, then add a measured amount of water.

8) Stir with a glass rod for about 3 to 4 minutes. The mixture will slowly thicken to a wet paste.

9) For every box of pills used, add:
- 1.0 g corn starch

10) Stir for a few minutes. The mixture will become very stiff and the consistency of damp potting soil, with no signs of visible liquid. Add more cornstarch in very small increments if necessary.

Why the cornstarch? The cornstarch is a great absorbent and helps to dry our mixture fast. When drying the cornstarch will keep our mixture from turning into hard little rocks and when powdered again keeps the mixture free flowing. It also will help absorb waxy gak when we extract our free base.

11) Spread out the mixture on the pie plate(s) and let dry completely. It will dry fast because the carbon has increased the surface area of our mixture.

12) When completely dry sift the mixture back into the beaker using the wire mesh strainer placed inside a large funnel.

13) For every box of pills used, add:
- 35 mL Naphtha

14) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a few minutes.

Isn't boiling naphtha dangerous? Boiling any flammable solvent is an extremely dangerous practice. Solvents should not be heated over an open flame or on any apparatus that is capable of producing a spark. This includes defective or damaged electric hot plates. Adequate ventilation is required. This should not be done in a closed environment due to risk of explosion and/or fire and due to health concerns regarding inhalation of solvent fumes. The constant use of a fan positioned to blow across the solvent will disburse the vapor, reduce the risk of fire and explosion.

15) While waiting, make a Charmin filter. Take 4 plys of Charmin and fold three times to make a square. Fold that over once and then once again to make a quarter square. Completely wet the square with some clean naphtha using the medicine dropper and place the pad into the bottom of the funnel across the neck. The Charmin should not be "packed" or "compressed". Gently mold the edges around the contour of the funnel bottom. Wet it again with naphtha and place this filter-funnel into the Erlenmeyer flask.

16) Slowly decant the naphtha into the funnel in small amounts and allow it to filter through the Charmin into the flask. Don't pour in more than can pass through the Charmin in more or less real time. If you make a big puddle it may start to crystallize in the funnel, clogging the filter. The filtered naphtha should be crystal clear. Free base crystals will start to form in the filtrate. Set the flask aside.

17) For every box of pills used, add:
- 20 mL Naphtha

18) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a minute.

19) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Don't pour in more than can pass through the Charmin in more or less real time. Do not replace the Charmin, continue to re-use the same pad.

20) For every box of pills used add:
- 10 mL Naphtha

21) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate.

22) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Then empty the entire contents of the beaker into the filter funnel and let drain.

23) While draining, boil a small amount of naphtha, about 5 mL for every box of pills used. When all the liquid appears to have drained through, pour the boiling naphtha over the filter cake and let it drain again. Then take a large spoon and press down on top of filter cake, squeezing any remaining naphtha into the flask.

Should I do a fourth pull? You can try but tests have shown it's usually not enough gain to justify the effort. Only do additional pulls if the end result is less than 45 %.

24) Place the Erlenmeyer flask with the combined filtrate on the hot plate set to med high. Heat to boiling or until all crystals have re-dissolved. Pour the hot filtrate into clean pie plate(s).

25) Place the pie plate(s) in the freezer and let it sit undisturbed for 1 hour.

26) Remove the pie plate(s) from the freezer and pour off the used naphtha, filtering out free base crystals using a coffee filter. Let the collected free base crystals dry. Some crystals may adhere to the pie plate. Let them dry before removing.

27) After filtering crystals out, return the used naphtha to the beaker. Return all filtered solids, including the Charmin filter, to the beaker. Break solids up with a glass rod and mix well. Return to hot plate on med high heat. With constant gentle stirring, bring the used mixture back to boiling. Let boil for 1 minute. Turn heat off but leave beaker on hot plate. Make a new Charmin filter as per previous step 15. Filter liquid first, then add remaining solids to funnel to drain. Then take a large spoon and press down on top of rhe filter cake, squeezing any remaining naphtha into the flask. Place into freezer again for at least 30 minutes. You can assemble a few extra percent. It helped recover one botched batch that would've been poor otherwise.

28) The remaining naphtha does contain some additional pseudoephedrine free base. You may wash the naphtha thoroughly with warm distilled water and titrate to obtain the remaining pseudoephedrine in HCL form. This pseudoephedrine HCL will not be as clean as the free base, and will need to be rinsed with acetone, then recrystallized twice before being added to a reaction. The use of this pseudoephedrine with the free base is not recommended. This pseudoephedrine HCl can be accumulated until the quantity is sufficient to react by itself.

29) If the HCl salt is the desired outcome, redissolve the free base crystals in to a nonpolar and gas accordingly. Do Not gas the original Naphtha. If you gas the original naphtha, you will pick up unwanted contaminants. You may alternatively move the free base crystals into a small quantity of distilled H2O, and add HCl drop wise with stirring until the free base crystals all dissolve. Evaporate over low heat until this alligators over, then flash with dry acetone. Filter the acetone and pseudoehphedrine HCl through a coffee filter, rinse with acetone, allow drying.

Calculating Yield

When calculating your yield, remember to adjust for free base. Pseudo HCl is about 202 g per mole and pseudo free base is about 166 g per mole. So 166 divided by 202 is a ratio of 0.82 So, potential yield from 1 box of 120's would be 20 x 120 x 0.82 = 1.9 g free base vs 2.4 g for pseudo HCl.

Advantages and Disadvantages

The technique should be, in the near future, virtually universal. It should successfully extract most pseudoephedrine pills. The materials are easily available and draw less attention than xylene and tolulene purchases. Yields should range in the sixty percent range. The pseudoephedrine so obtained will be very clean-characteristic of A/B extractions of pseudoephedrine. The main disadvantage is heating a flammable solvent.

Time

You can run it in about 3 hours start to finish, 4 hours with the fourth pull. The first few times I would allow 5 hours to be safe until you get the feel of it. Each box of pills used has the potential of 1.9 g of free base. This is equivalent to 2.4 g of the HCL salt.
具有良好实验室技能的普通化学家应该能够始终如一地获得每盒 1 克超洁净游离碱,即 52%。
具有良好实验室技能的经验丰富的化学家应该能够始终如一地实现每盒 1.2 克超清洁游离碱,或者 63 - 65% 似乎是当前形式的墙,但我们正在研究一些解决方案。

结晶可以采取两种不同的形式
快速方法:将热石脑油立即放入冰箱而不冷却,通常会产生细小的雪状晶体。
如果你不着急: 让石脑油冷却到室温左右,然后放入冰箱,你通常会得到像这样的大而闪闪发光的美丽。


方法2

概括

一种从不断变化的药丸中以高产率生产清洁假盐酸的新方法。它不仅像上面的方法那样少水,而且更简单,根本没有 A/B。这是方法2或直接提取。这是一种简单的提取方法,可以绕过当今大多数的现代掺假物,并返回非常高产率的干净的假HCl。然后可以将其重结晶或转化为游离碱以生产原始产品。该方法的编写是为了易于扩展,而且非常方便。清洁伪 HCl 的平均产率为 80% 至 90% 。

设备和玻璃器皿

  • 三个烧杯或其他耐热玻璃器皿容器(每盒药丸约200毫升)
  • 一个elemeyer烧瓶或其他耐热玻璃器皿容器(每盒药丸约200毫升)
  • 1 个量筒 100 -200 mL 或其他液体测量装置(以 mL 为单位)
  • 两个 5" 玻璃漏斗或塑料燃料漏斗
  • 滤纸或咖啡滤纸
  • 玻璃搅拌棒或竹串
  • 热板
  • 小风扇
  • 小规模称量(克)
  • 安全眼镜、乳胶手套
  • 温度计的刻度至少为 120°C

试剂:

  • 91- 99% 异丙醇(药店有售)
  • MEK 甲基乙基酮(油漆/五金店)
  • VM&P 石脑油 - 无替代品(油漆/五金店)
  • (请勿使用 Colemans、石油醚、打火机油等)
  • 二甲苯(油漆/五金店)

干燥助剂:

  • 烘干泻盐或洗涤苏打(药店/食品店)
  • 盐(食品店)

程序摘要

  1. 制作萃取液。
  2. 将整个药丸放入烧杯中。
  3. 添加萃取液。
  4. 加热至沸腾,搅拌直至药丸溶解。
  5. 趁热过滤至 elemeyer 烧瓶中。
  6. 重复两次。
  7. 将合并的萃取物返回到干净的烧杯中。
  8. 添加二甲苯
  9. 加热至105℃使酒精沸腾。
  10. 滤出假HCl。
  11. 用 MEK 清洗伪 HCl 并干燥。

程序
1)对于每盒所使用的药丸:将以下溶剂和干燥材料按以下顺序混合在干净的烧杯中:
70 毫升异丙醇
70 mL VM&P 石脑油
2克盐
4 克干泻盐或干洗涤苏打


2)用玻璃棒搅拌几分钟,然后静置10分钟。根据开始时异丙醇中的水含量,混合物将沉降成 2 层或 1 层,底部有潮湿固体。

为什么不首先使用预干燥的溶剂?- 如果你有它们,那就完全没问题,但我注意到,将异丙基和石脑油添加在一起几乎总是会释放一些水,无论它们提前有多干燥,所以我不会跳过这一步。

3)将其过滤到elemeyer烧瓶中,留下任何固体或底部液体层,然后将该溶液转移到第二个干净的烧杯中。

4)将整粒药片放入第三个干净的烧杯中。

为什么是整粒药?我不需要先把它们磨碎吗?- 不,我们正在努力将损失降至最低,并且不需要研磨,因为异丙基/石脑油混合物会很好地溶解它们。

5)将 1/3 溶剂混合物倒在药丸上。

6)将烧杯放在电炉上,用中火煮沸。使用小风扇防止蒸汽积聚。偶尔用玻璃棒搅拌,直到药丸溶解成粉末。煮1-2分钟。

7)将带有滤纸的漏斗放入elemeyer烧瓶中。趁热过滤溶剂混合物,将尽可能多的固体留在烧杯中。

8)将所有固体返回烧杯并重复步骤 5 至 7 两次,将萃取物合并到 elemeyer 烧瓶中。

9)对于每盒使用的药丸,添加到合并的提取物中:
- 50 毫升二甲苯

10)将萃取混合物转移回空溶剂烧杯中,并将烧杯放在电炉上。使用小风扇将其煮沸,以防止蒸汽积聚。煮沸直至溶液达到 105 °C。

11)使用干净的漏斗和过滤器,趁溶液热时滤去假HCl。

12)用大量 MEK 冲洗漏斗中的假 HCl。

13)从漏斗中取出过滤器和滤饼并使其完全干燥。(不再有 MEK 气味)

Introduction

It is totally OTC and uses activated carbon as a cleaning aide while exploiting characteristics of VM&P naphtha. Average yield is 60 % of very clean free base.

Definitions
In this write-up will be used the phrase "for every box of pills used". This stands for every box of 48 x 60 mg, or 96 x 30 mg, or 20 x 120 mg. In addition, the phrase "for every gram of total pill mass" will be used. This stands for the total weight of the pills before grinding.

Method 1

Equipment and glassware:

  • One beaker or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One erlenmeyer flask or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One graduated cylinder 100-200 mL or other liquid measuring device in mL
  • One pyrex pie plate (2 if more than 5 boxes are used)
  • Two 5" glass funnels or plastic fuel funnels
  • One 5" wire mesh kitchen strainer (dollar store type)
  • One 5 mL baby medicine dropper
  • Charmin bath tissue (reg no scent)
  • Glass stirring rod or bamboo skewers
  • Clean coffee grinder
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
Reagents:
  • Activated carbon, research grade (pets fart store)
  • Corn starch (supermarket)
  • Dry acetone - CH3COCH3 (dried with baked sodium carbonate)
  • Sodium carbonate - Na2CO3 (washing soda)
  • Sodium chloride - NaCl (salt)
  • Sodium hydroxide - NaOH (lye)
  • VM&P naphtha - no substitutions (paint store), do Not use colemans, pet ether, lighter fluid, etc.
Optional Materials:
Gassing setup if HCl salt is desired outcome

Abstract of Procedure:

  1. Combine Pills with activated carbon, NaCl, NaOH and Na2CO3.
  2. Grind to a fine powder and sift through strainer.
  3. Stir in acetone.
  4. Add a trace amount of water.
  5. Mix until paste.
  6. Add corn starch.
  7. Mix until consistency of damp potting soil.
  8. Dry completely.
  9. Add naphtha.
  10. Heat to boiling while stirring.
  11. Filter thru Charmin filter.
  12. Repeat two times
  13. Freeze filtrate.
  14. Filter out crystals.
  15. Convert to salt form if desired.

Procedure

1) Weigh pills and record total weight.

2) Place pills into a clean coffee grinder.

3) For every box of pills used, add:
- 2 g of washing soda
- 2 g of salt
- 4 g of activated carbon
- 4 g sodium hydroxide


What if it all won't fit in the coffee grinder. Process about 3 - 4 boxes at a time.
Why am I adding salt? To attract water and to act as an abrasive to aid in grinding.
Why am I adding washing soda? To act as a buffering agent.


After grinding, the mixture becomes hot and doesn't sift well? Carbon sold for aquarium filtration may contain excess moisture. The moisture content will be apparent when the carbon is ground. Moist carbon will tend to cake on the side of the grinder, and will feel moist. If the carbon is moist, dry it before use by heating in an oven or microwave. Take precautions handling the heated carbon to avoid burns. Allow the carbon to cool before grinding or combining with other ingredients. Store any unused dried carbon in an airtight container.

4) Grind the mixture to a fine powder. It is important that we grind the mixture as fine and uniformly as possible, about the consistency of coarse flour.

5) Sift the mixture into the beaker using a wire mesh strainer placed inside a large funnel to minimize dusting. When grinding and sifting, be careful with vents, fans and open windows, so your pseudo doesn't blow away as dust. You also don't want to inhale NaOH or carbon dust. Let the dust settle in the coffee grinder before opening the lid.

6) For every gram of total pill mass, add:
- 1.5 mL dry acetone

This measurement will get you in the ballpark. We want the mixture to be a liquid at this point, not a paste. Add more acetone in small increments, as the mixture will go from stiff to fluid very quickly. Acetone used for this purpose should be dried before use, as the moisture content of acetone can vary over such a wide range that the only way to obtain consistent results it to dry the acetone before use.

7) For every box of pills used add, while stirring:
- 3 drops distilled H2O (use the baby medicine dropper)

Why are we using dry acetone and then adding water? Since the amount of moisture present is critical for proper basing, and the water content of non-dried acetone is widely variable, the only way to accurately control the moisture available for basing is to dry the acetone first, then add a measured amount of water.

8) Stir with a glass rod for about 3 to 4 minutes. The mixture will slowly thicken to a wet paste.

9) For every box of pills used, add:
- 1.0 g corn starch

10) Stir for a few minutes. The mixture will become very stiff and the consistency of damp potting soil, with no signs of visible liquid. Add more cornstarch in very small increments if necessary.

Why the cornstarch? The cornstarch is a great absorbent and helps to dry our mixture fast. When drying the cornstarch will keep our mixture from turning into hard little rocks and when powdered again keeps the mixture free flowing. It also will help absorb waxy gak when we extract our free base.

11) Spread out the mixture on the pie plate(s) and let dry completely. It will dry fast because the carbon has increased the surface area of our mixture.

12) When completely dry sift the mixture back into the beaker using the wire mesh strainer placed inside a large funnel.

13) For every box of pills used, add:
- 35 mL Naphtha

14) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a few minutes.

Isn't boiling naphtha dangerous? Boiling any flammable solvent is an extremely dangerous practice. Solvents should not be heated over an open flame or on any apparatus that is capable of producing a spark. This includes defective or damaged electric hot plates. Adequate ventilation is required. This should not be done in a closed environment due to risk of explosion and/or fire and due to health concerns regarding inhalation of solvent fumes. The constant use of a fan positioned to blow across the solvent will disburse the vapor, reduce the risk of fire and explosion.

15) While waiting, make a Charmin filter. Take 4 plys of Charmin and fold three times to make a square. Fold that over once and then once again to make a quarter square. Completely wet the square with some clean naphtha using the medicine dropper and place the pad into the bottom of the funnel across the neck. The Charmin should not be "packed" or "compressed". Gently mold the edges around the contour of the funnel bottom. Wet it again with naphtha and place this filter-funnel into the Erlenmeyer flask.

16) Slowly decant the naphtha into the funnel in small amounts and allow it to filter through the Charmin into the flask. Don't pour in more than can pass through the Charmin in more or less real time. If you make a big puddle it may start to crystallize in the funnel, clogging the filter. The filtered naphtha should be crystal clear. Free base crystals will start to form in the filtrate. Set the flask aside.

17) For every box of pills used, add:
- 20 mL Naphtha

18) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a minute.

19) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Don't pour in more than can pass through the Charmin in more or less real time. Do not replace the Charmin, continue to re-use the same pad.

20) For every box of pills used add:
- 10 mL Naphtha

21) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate.

22) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Then empty the entire contents of the beaker into the filter funnel and let drain.

23) While draining, boil a small amount of naphtha, about 5 mL for every box of pills used. When all the liquid appears to have drained through, pour the boiling naphtha over the filter cake and let it drain again. Then take a large spoon and press down on top of filter cake, squeezing any remaining naphtha into the flask.

Should I do a fourth pull? You can try but tests have shown it's usually not enough gain to justify the effort. Only do additional pulls if the end result is less than 45 %.

24) Place the Erlenmeyer flask with the combined filtrate on the hot plate set to med high. Heat to boiling or until all crystals have re-dissolved. Pour the hot filtrate into clean pie plate(s).

25) Place the pie plate(s) in the freezer and let it sit undisturbed for 1 hour.

26) Remove the pie plate(s) from the freezer and pour off the used naphtha, filtering out free base crystals using a coffee filter. Let the collected free base crystals dry. Some crystals may adhere to the pie plate. Let them dry before removing.

27)滤出晶体后,将用过的石脑油返回烧杯中。将所有过滤的固体(包括 Charmin 过滤器)返回到烧杯中。用玻璃棒打碎固体并充分混合。返回到中高温的热板上。持续温和搅拌,使用过的混合物重新沸腾。煮1分钟。关掉热量,但将烧杯放在热板上。按照之前的步骤 15 制作新的 Charmin 过滤器。首先过滤液体,然后将剩余的固体添加到漏斗中以排出。然后拿一个大勺子压在滤饼顶部,将剩余的石脑油挤入烧瓶中。再次放入冰箱冷藏至少30分钟。你可以多凑几个百分点。它帮助恢复了一批质量较差的产品,否则这些产品的质量就会很差。

28)剩余的石脑油确实含有一些额外的伪麻黄碱游离碱。您可以用温蒸馏水彻底洗涤石脑油并滴定以获得剩余的 HCL 形式的伪麻黄碱。这种伪麻黄碱盐酸盐不像游离碱那么干净,需要用丙酮冲洗,然后重结晶两次,然后再添加到反应中。不建议将这种伪麻黄碱与游离碱一起使用。这种盐酸伪麻黄碱可以积累,直到其数量足以自行反应。

29)如果 HCl 盐是所需的结果,则将游离碱晶体重新溶解成相应的非极性气体。不要用原始石脑油进行气化。如果对原始石脑油进行气体处理,则会吸收不需要的污染物。您也可以将游离碱晶体移入少量蒸馏水中,并在搅拌下滴加 HCl,直至游离碱晶体全部溶解。用小火蒸发直至鳄鱼消失,然后用干燥丙酮进行闪蒸。通过咖啡过滤器过滤丙酮和盐酸伪麻黄碱,用丙酮冲洗,干燥。

计算产量

计算收益时,请记住根据免费基础进行调整。假HCl约为每摩尔202克,假游离碱约为每摩尔166克。因此 166 除以 202 的比率为 0.82 因此,一盒 120 的潜在产量将为 20 x 120 x 0.82 = 1.9 g 游离碱,而假 HCl 则为 2.4 g。

的优点和缺点

在不久的将来,这项技术应该几乎普及。它应该能成功提取大多数伪麻黄碱药丸。这些材料很容易获得,并且不像二甲苯和甲苯那样引起人们的关注。收益率应在百分之六十范围内。如此获得的伪麻黄碱将具有非常纯净的伪麻黄碱A/B提取物特征。主要缺点是加热易燃溶剂。

时间

从开始到结束大约需要 3 小时,第四次拉动需要 4 小时。最初几次,我会留出 5 个小时的时间来保证安全,直到你找到感觉为止。每盒所用药丸可能含有 1.9 克游离碱。这相当于 2.4 克 HCL 盐。
具有良好实验室技能的普通化学家应该能够始终如一地获得每盒 1 克超洁净游离碱,即 52%。
具有良好实验室技能的经验丰富的化学家应该能够始终如一地实现每盒 1.2 克超清洁游离碱,或者 63 - 65% 似乎是当前形式的墙,但我们正在研究一些解决方案。

结晶可以采取两种不同的形式
快速方法:将热石脑油立即放入冰箱而不冷却,通常会产生细小的雪状晶体。
如果你不着急: 让石脑油冷却到室温左右,然后放入冰箱,你通常会得到像这样的大而闪闪发光的美丽。


方法2

概括

一种从不断变化的药丸中以高产率生产清洁假盐酸的新方法。它不仅像上面的方法那样少水,而且更简单,根本没有 A/B。这是方法2或直接提取。这是一种简单的提取方法,可以绕过当今大多数的现代掺假物,并返回非常高产率的干净的假HCl。然后可以将其重结晶或转化为游离碱以生产原始产品。该方法的编写是为了易于扩展,而且非常方便。清洁伪 HCl 的平均产率为 80% 至 90% 。

设备和玻璃器皿

  • 三个烧杯或其他耐热玻璃器皿容器(每盒药丸约200毫升)
  • 一个elemeyer烧瓶或其他耐热玻璃器皿容器(每盒药丸约200毫升)
  • 1 个量筒 100 -200 mL 或其他液体测量装置(以 mL 为单位)
  • 两个 5" 玻璃漏斗或塑料燃料漏斗
  • 滤纸或咖啡滤纸
  • 玻璃搅拌棒或竹串
  • 热板
  • 小风扇
  • 小规模称量(克)
  • 安全眼镜、乳胶手套
  • 温度计的刻度至少为 120°C

试剂:

  • 91- 99% 异丙醇(药店有售)
  • MEK 甲基乙基酮(油漆/五金店)
  • VM&P 石脑油 - 无替代品(油漆/五金店)
  • (请勿使用 Colemans、石油醚、打火机油等)
  • 二甲苯(油漆/五金店)

干燥助剂:

  • 烘干泻盐或洗涤苏打(药店/食品店)
  • 盐(食品店)

程序摘要

  1. 制作萃取液。
  2. 将整个药丸放入烧杯中。
  3. 添加萃取液。
  4. 加热至沸腾,搅拌直至药丸溶解。
  5. 趁热过滤至 elemeyer 烧瓶中。
  6. 重复两次。
  7. 将合并的萃取物返回到干净的烧杯中。
  8. 添加二甲苯
  9. 加热至105℃使酒精沸腾。
  10. 滤出假HCl。
  11. 用 MEK 清洗伪 HCl 并干燥。

程序
1)对于每盒所使用的药丸:将以下溶剂和干燥材料按以下顺序混合在干净的烧杯中:
70 毫升异丙醇
70 mL VM&P 石脑油
2克盐
4 克干泻盐或干洗涤苏打


2)用玻璃棒搅拌几分钟,然后静置10分钟。根据开始时异丙醇中的水含量,混合物将沉降成 2 层或 1 层,底部有潮湿固体。

为什么不首先使用预干燥的溶剂?- 如果你有它们,那就完全没问题,但我注意到,将异丙基和石脑油添加在一起几乎总是会释放一些水,无论它们提前有多干燥,所以我不会跳过这一步。

3)将其过滤到elemeyer烧瓶中,留下任何固体或底部液体层,然后将该溶液转移到第二个干净的烧杯中。

4)将整粒药片放入第三个干净的烧杯中。

为什么是整粒药?我不需要先把它们磨碎吗?- 不,我们正在努力将损失降至最低,并且不需要研磨,因为异丙基/石脑油混合物会很好地溶解它们。

5)将 1/3 溶剂混合物倒在药丸上。

6)将烧杯放在电炉上,用中火煮沸。使用小风扇防止蒸汽积聚。偶尔用玻璃棒搅拌,直到药丸溶解成粉末。煮1-2分钟。

7)将带有滤纸的漏斗放入elemeyer烧瓶中。趁热过滤溶剂混合物,将尽可能多的固体留在烧杯中。

8)将所有固体返回烧杯并重复步骤 5 至 7 两次,将萃取物合并到 elemeyer 烧瓶中。

9)对于每盒使用的药丸,添加到

G.Patton

Introduction

It is totally OTC and uses activated carbon as a cleaning aide while exploiting characteristics of VM&P naphtha. Average yield is 60 % of very clean free base.

Definitions
In this write-up will be used the phrase "for every box of pills used". This stands for every box of 48 x 60 mg, or 96 x 30 mg, or 20 x 120 mg. In addition, the phrase "for every gram of total pill mass" will be used. This stands for the total weight of the pills before grinding.

Method 1

Equipment and glassware:

  • One beaker or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One erlenmeyer flask or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One graduated cylinder 100-200 mL or other liquid measuring device in mL
  • One pyrex pie plate (2 if more than 5 boxes are used)
  • Two 5" glass funnels or plastic fuel funnels
  • One 5" wire mesh kitchen strainer (dollar store type)
  • One 5 mL baby medicine dropper
  • Charmin bath tissue (reg no scent)
  • Glass stirring rod or bamboo skewers
  • Clean coffee grinder
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
Reagents:
  • Activated carbon, research grade (pets fart store)
  • Corn starch (supermarket)
  • Dry acetone - CH3COCH3 (dried with baked sodium carbonate)
  • Sodium carbonate - Na2CO3 (washing soda)
  • Sodium chloride - NaCl (salt)
  • Sodium hydroxide - NaOH (lye)
  • VM&P naphtha - no substitutions (paint store), do Not use colemans, pet ether, lighter fluid, etc.
Optional Materials:
Gassing setup if HCl salt is desired outcome

Abstract of Procedure:

  1. Combine Pills with activated carbon, NaCl, NaOH and Na2CO3.
  2. Grind to a fine powder and sift through strainer.
  3. Stir in acetone.
  4. Add a trace amount of water.
  5. Mix until paste.
  6. Add corn starch.
  7. Mix until consistency of damp potting soil.
  8. Dry completely.
  9. Add naphtha.
  10. Heat to boiling while stirring.
  11. Filter thru Charmin filter.
  12. Repeat two times
  13. Freeze filtrate.
  14. Filter out crystals.
  15. Convert to salt form if desired.

Procedure

1) Weigh pills and record total weight.

2) Place pills into a clean coffee grinder.

3) For every box of pills used, add:
- 2 g of washing soda
- 2 g of salt
- 4 g of activated carbon
- 4 g sodium hydroxide


What if it all won't fit in the coffee grinder. Process about 3 - 4 boxes at a time.
Why am I adding salt? To attract water and to act as an abrasive to aid in grinding.
Why am I adding washing soda? To act as a buffering agent.


After grinding, the mixture becomes hot and doesn't sift well? Carbon sold for aquarium filtration may contain excess moisture. The moisture content will be apparent when the carbon is ground. Moist carbon will tend to cake on the side of the grinder, and will feel moist. If the carbon is moist, dry it before use by heating in an oven or microwave. Take precautions handling the heated carbon to avoid burns. Allow the carbon to cool before grinding or combining with other ingredients. Store any unused dried carbon in an airtight container.

4) Grind the mixture to a fine powder. It is important that we grind the mixture as fine and uniformly as possible, about the consistency of coarse flour.

5) Sift the mixture into the beaker using a wire mesh strainer placed inside a large funnel to minimize dusting. When grinding and sifting, be careful with vents, fans and open windows, so your pseudo doesn't blow away as dust. You also don't want to inhale NaOH or carbon dust. Let the dust settle in the coffee grinder before opening the lid.

6) For every gram of total pill mass, add:
- 1.5 mL dry acetone

This measurement will get you in the ballpark. We want the mixture to be a liquid at this point, not a paste. Add more acetone in small increments, as the mixture will go from stiff to fluid very quickly. Acetone used for this purpose should be dried before use, as the moisture content of acetone can vary over such a wide range that the only way to obtain consistent results it to dry the acetone before use.

7) For every box of pills used add, while stirring:
- 3 drops distilled H2O (use the baby medicine dropper)

Why are we using dry acetone and then adding water? Since the amount of moisture present is critical for proper basing, and the water content of non-dried acetone is widely variable, the only way to accurately control the moisture available for basing is to dry the acetone first, then add a measured amount of water.

8) Stir with a glass rod for about 3 to 4 minutes. The mixture will slowly thicken to a wet paste.

9) For every box of pills used, add:
- 1.0 g corn starch

10) Stir for a few minutes. The mixture will become very stiff and the consistency of damp potting soil, with no signs of visible liquid. Add more cornstarch in very small increments if necessary.

Why the cornstarch? The cornstarch is a great absorbent and helps to dry our mixture fast. When drying the cornstarch will keep our mixture from turning into hard little rocks and when powdered again keeps the mixture free flowing. It also will help absorb waxy gak when we extract our free base.

11) Spread out the mixture on the pie plate(s) and let dry completely. It will dry fast because the carbon has increased the surface area of our mixture.

12) When completely dry sift the mixture back into the beaker using the wire mesh strainer placed inside a large funnel.

13) For every box of pills used, add:
- 35 mL Naphtha

14) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a few minutes.

Isn't boiling naphtha dangerous? Boiling any flammable solvent is an extremely dangerous practice. Solvents should not be heated over an open flame or on any apparatus that is capable of producing a spark. This includes defective or damaged electric hot plates. Adequate ventilation is required. This should not be done in a closed environment due to risk of explosion and/or fire and due to health concerns regarding inhalation of solvent fumes. The constant use of a fan positioned to blow across the solvent will disburse the vapor, reduce the risk of fire and explosion.

15) While waiting, make a Charmin filter. Take 4 plys of Charmin and fold three times to make a square. Fold that over once and then once again to make a quarter square. Completely wet the square with some clean naphtha using the medicine dropper and place the pad into the bottom of the funnel across the neck. The Charmin should not be "packed" or "compressed". Gently mold the edges around the contour of the funnel bottom. Wet it again with naphtha and place this filter-funnel into the Erlenmeyer flask.

16) Slowly decant the naphtha into the funnel in small amounts and allow it to filter through the Charmin into the flask. Don't pour in more than can pass through the Charmin in more or less real time. If you make a big puddle it may start to crystallize in the funnel, clogging the filter. The filtered naphtha should be crystal clear. Free base crystals will start to form in the filtrate. Set the flask aside.

17) For every box of pills used, add:
- 20 mL Naphtha

18) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a minute.

19) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Don't pour in more than can pass through the Charmin in more or less real time. Do not replace the Charmin, continue to re-use the same pad.

20) For every box of pills used add:
- 10 mL Naphtha

21) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate.

22) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Then empty the entire contents of the beaker into the filter funnel and let drain.

23) While draining, boil a small amount of naphtha, about 5 mL for every box of pills used. When all the liquid appears to have drained through, pour the boiling naphtha over the filter cake and let it drain again. Then take a large spoon and press down on top of filter cake, squeezing any remaining naphtha into the flask.

Should I do a fourth pull? You can try but tests have shown it's usually not enough gain to justify the effort. Only do additional pulls if the end result is less than 45 %.

24) Place the Erlenmeyer flask with the combined filtrate on the hot plate set to med high. Heat to boiling or until all crystals have re-dissolved. Pour the hot filtrate into clean pie plate(s).

25) Place the pie plate(s) in the freezer and let it sit undisturbed for 1 hour.

26) Remove the pie plate(s) from the freezer and pour off the used naphtha, filtering out free base crystals using a coffee filter. Let the collected free base crystals dry. Some crystals may adhere to the pie plate. Let them dry before removing.

27) After filtering crystals out, return the used naphtha to the beaker. Return all filtered solids, including the Charmin filter, to the beaker. Break solids up with a glass rod and mix well. Return to hot plate on med high heat. With constant gentle stirring, bring the used mixture back to boiling. Let boil for 1 minute. Turn heat off but leave beaker on hot plate. Make a new Charmin filter as per previous step 15. Filter liquid first, then add remaining solids to funnel to drain. Then take a large spoon and press down on top of rhe filter cake, squeezing any remaining naphtha into the flask. Place into freezer again for at least 30 minutes. You can assemble a few extra percent. It helped recover one botched batch that would've been poor otherwise.

28) The remaining naphtha does contain some additional pseudoephedrine free base. You may wash the naphtha thoroughly with warm distilled water and titrate to obtain the remaining pseudoephedrine in HCL form. This pseudoephedrine HCL will not be as clean as the free base, and will need to be rinsed with acetone, then recrystallized twice before being added to a reaction. The use of this pseudoephedrine with the free base is not recommended. This pseudoephedrine HCl can be accumulated until the quantity is sufficient to react by itself.

29) If the HCl salt is the desired outcome, redissolve the free base crystals in to a nonpolar and gas accordingly. Do Not gas the original Naphtha. If you gas the original naphtha, you will pick up unwanted contaminants. You may alternatively move the free base crystals into a small quantity of distilled H2O, and add HCl drop wise with stirring until the free base crystals all dissolve. Evaporate over low heat until this alligators over, then flash with dry acetone. Filter the acetone and pseudoehphedrine HCl through a coffee filter, rinse with acetone, allow drying.

Calculating Yield

When calculating your yield, remember to adjust for free base. Pseudo HCl is about 202 g per mole and pseudo free base is about 166 g per mole. So 166 divided by 202 is a ratio of 0.82 So, potential yield from 1 box of 120's would be 20 x 120 x 0.82 = 1.9 g free base vs 2.4 g for pseudo HCl.

Advantages and Disadvantages

The technique should be, in the near future, virtually universal. It should successfully extract most pseudoephedrine pills. The materials are easily available and draw less attention than xylene and tolulene purchases. Yields should range in the sixty percent range. The pseudoephedrine so obtained will be very clean-characteristic of A/B extractions of pseudoephedrine. The main disadvantage is heating a flammable solvent.

Time

You can run it in about 3 hours start to finish, 4 hours with the fourth pull. The first few times I would allow 5 hours to be safe until you get the feel of it. Each box of pills used has the potential of 1.9 g of free base. This is equivalent to 2.4 g of the HCL salt.
The average chemist with fair lab skills should be able to consistently achieve 1 gram of super clean free base per box, or 52%.
The experienced chemist with good lab skills should be able to consistently achieve 1.2 g of super clean free base per box or 63 - 65% seems to be the wall in its current form, but we're working on a few solutions.

Crystallization can take two different forms
The fast way: Placing the hot naphtha immediately in the freezer with no cool down will generally produce fine snow like crystals.
If you're not in a hurry: let the naphtha cool to about room temperature before placing into the freezer, and you will generally get large sparkling beauties like these.


Method 2

Summary

A new twist for producing clean pseudo HCl in high yields from an ever-changing array of pills. It's not only water less like in method above, it's simpler with no A/B at all. It's Method 2 or straight to the extraction. It is a simple extraction method that will bypass most of today’s modern adulterants and will return a very high yield of clean pseudo HCl. This can then be recrystallized or turned into free base to produce a pristine product. This method was written to be easily scalable and is very over the counter. Average yields have been 80 % to 90 % of clean pseudo HCl.

Equipment and glassware:

  • Three beakers or other heatproof glassware containers (approximately 200ml for every box of pills used)
  • One elemeyer flask or other heatproof glassware container (approximately 200ml for every box of pills used)
  • One graduated cylinder 100 -200 mL or other liquid measuring device in mLs
  • Two 5" glass funnels or plastic fuel funnels
  • Filter Paper or coffee filters
  • Glass stirring rod or bamboo skewers
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
  • Thermometer that is scaled to at least 120°C

Reagents:

  • 91- 99% Isopropyl Alcohol (drug store)
  • MEK Methyl Ethyl Ketone (paint / hardware store)
  • VM&P Naphtha - no substitutions (paint / hardware store)
  • (Do Not use Colemans, pet ether, lighter fluid, etc.)
  • Xylene (paint / hardware store)

Drying Aids:

  • Oven dried Epsom Salts or Washing Soda (drug / food store)
  • Salt (food store)

Abstract of Procedure

  1. Make extraction fluid.
  2. Place whole pills into beaker.
  3. Add extraction fluid.
  4. Heat to boiling, stirring until pills dissolve.
  5. Filter while hot into elemeyer flask.
  6. Repeat two times.
  7. Return combined extractions to clean beaker.
  8. Add Xylene
  9. Heat to 105 °C to boil off alcohol.
  10. Filter out pseudo HCl.
  11. Wash pseudo HCl with MEK and let dry.

Procedure
1) For every box of pills used: combine the following solvents and drying materials in a clean beaker and in the following order:
70 mL Isopropyl Alcohol
70 mL VM&P Naphtha
2 g of salt
4 g of dried epsom salts or dried washing soda


2) Stir with a glass rod for a few minutes, then let settle for 10 minutes. Depending on how much water was in the isopropyl alcohol to start with, the mixture will settle into 2 layers or 1 layer with damp solids at the bottom.

Why not use pre dried solvents to begin with? - that is perfectly ok if you have them, but I have noticed that adding the isopropyl and naphtha together almost always releases some water, no matter how dry they were ahead of time, so I would not skip this step.

3) Filter this into the elemeyer flask leaving any solids or bottom liquid layer behind and then transfer this solution into the second clean beaker.

4) Place whole pills in the third clean beaker.

Why whole pills? Don’t I need to grind them up first? - no, we are trying to keep loss to a minimum and grinding is not necessary as the isopropyl / naphtha mixture will dissolve them very well.

5) Pour 1/3 solvent mixture over pills.

6) Place the beaker on the hotplate and bring to a boil using medium hi heat. Use the small fan to keep vapors from accumulating. Stir occasionally with a glass rod until pills have dissolved into powder. Let boil for 1-2 minutes.

7) Place a funnel with filter paper in the elemeyer flask. Filter the solvent mixture while hot, leaving as much of the solids in the beaker as possible.

8) Return any solids to the beaker and repeat steps 5 through 7 two times, combining the extractions in the elemeyer flask.

9) For every box of pills used, add to the combined extractions:
- 50 mL Xylene

10) Transfer the extraction mixture back to the empty solvent beaker and place the beaker on the hotplate. Bring to a boil using the small fan to keep vapors from accumulating. Boil until the solution reaches 105 °C.

11) Using a clean funnel and filter, paper filter off the pseudo HCl while the solution is hot.

12) Rinse the pseudo HCl with a generous amount of MEK while in the funnel.

13) Remove filter and filter cake from funnel and allow to dry completely. (no more MEK smell)

14) Weight and enjoy, yield should be between 80 % to 90 % Introduction
Hello, Patton, in method two, can acetone be used instead of methyl ethyl ketone? Can xylene be replaced with toluene? Can you show me a picture of the pseudoephedrine hydrochloride extracted from the pills? At one point I had an extract that was like fiberglass, but I'm not sure that was it.
 
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G.Patton

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Hello, Patton, in method two, can acetone be used instead of methyl ethyl ketone? Can xylene be replaced with toluene? Can you show me a picture of the pseudoephedrine hydrochloride extracted from the pills? At one point I had an extract that was like fiberglass, but I'm not sure that was it.
iceHello, I guess so
can acetone be used instead of methyl ethyl ketone?
Can xylene be replaced with toluene?

You can check its melting point to approve that it's ephedrine if you have doubts
At one point I had an extract that was like fiberglass, but I'm not sure that was it.
 

ice

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Hello, I guess so



You can check its melting point to approve that it's ephedrine if you have doubts
G.PattonThank you very much Patton. Yesterday I researched a pill and first dissolved it with ethanol. According to the information, I found that only pseudoephedrine hydrochloride, cetirizine hydrochloride, and hypromellose can be dissolved. I do get crystals. My current thought is to dissolve them with acetone, remove the cetirizine hydrochloride, and finally use hot water to remove the hypromellose. Is my approach feasible? Is pseudoephedrine hydrochloride soluble in acetone? Is hypromellose insoluble in hot water? If feasible, this pill extraction would be very convenient
 

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Hello, Patton, in method two, can acetone be used instead of methyl ethyl ketone? Can xylene be replaced with toluene? Can you show me a picture of the pseudoephedrine hydrochloride extracted from the pills? At one point I had an extract that was like fiberglass, but I'm not sure that was it.
iceWhat can I do if some of my activated charcoal made it through my filtering?? Redissolve and filter again?
 

zaners

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Hello, Patton, in method two, can acetone be used instead of methyl ethyl ketone? Can xylene be replaced with toluene? Can you show me a picture of the pseudoephedrine hydrochloride extracted from the pills? At one point I had an extract that was like fiberglass, but I'm not sure that was it.
iceIn the first method it says the left over napatha will have pseudoephedrine freebase in it so add water and "titrate"how do you titrate?
 

bigbadbear

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can I extract ephedrine from ephedrine syrup ?🤔🤔

Introduction

It is totally OTC and uses activated carbon as a cleaning aide while exploiting characteristics of VM&P naphtha. Average yield is 60 % of very clean free base.

Definitions
In this write-up will be used the phrase "for every box of pills used". This stands for every box of 48 x 60 mg, or 96 x 30 mg, or 20 x 120 mg. In addition, the phrase "for every gram of total pill mass" will be used. This stands for the total weight of the pills before grinding.

Method 1

Equipment and glassware:

  • One beaker or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One erlenmeyer flask or other heatproof glassware (approximately 100 mL for every box of pills used)
  • One graduated cylinder 100-200 mL or other liquid measuring device in mL
  • One pyrex pie plate (2 if more than 5 boxes are used)
  • Two 5" glass funnels or plastic fuel funnels
  • One 5" wire mesh kitchen strainer (dollar store type)
  • One 5 mL baby medicine dropper
  • Charmin bath tissue (reg no scent)
  • Glass stirring rod or bamboo skewers
  • Clean coffee grinder
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
Reagents:
  • Activated carbon, research grade (pets fart store)
  • Corn starch (supermarket)
  • Dry acetone - CH3COCH3 (dried with baked sodium carbonate)
  • Sodium carbonate - Na2CO3 (washing soda)
  • Sodium chloride - NaCl (salt)
  • Sodium hydroxide - NaOH (lye)
  • VM&P naphtha - no substitutions (paint store), do Not use colemans, pet ether, lighter fluid, etc.
Optional Materials:
Gassing setup if HCl salt is desired outcome

Abstract of Procedure:

  1. Combine Pills with activated carbon, NaCl, NaOH and Na2CO3.
  2. Grind to a fine powder and sift through strainer.
  3. Stir in acetone.
  4. Add a trace amount of water.
  5. Mix until paste.
  6. Add corn starch.
  7. Mix until consistency of damp potting soil.
  8. Dry completely.
  9. Add naphtha.
  10. Heat to boiling while stirring.
  11. Filter thru Charmin filter.
  12. Repeat two times
  13. Freeze filtrate.
  14. Filter out crystals.
  15. Convert to salt form if desired.

Procedure

1) Weigh pills and record total weight.

2) Place pills into a clean coffee grinder.

3) For every box of pills used, add:
- 2 g of washing soda
- 2 g of salt
- 4 g of activated carbon
- 4 g sodium hydroxide


What if it all won't fit in the coffee grinder. Process about 3 - 4 boxes at a time.
Why am I adding salt? To attract water and to act as an abrasive to aid in grinding.
Why am I adding washing soda? To act as a buffering agent.


After grinding, the mixture becomes hot and doesn't sift well? Carbon sold for aquarium filtration may contain excess moisture. The moisture content will be apparent when the carbon is ground. Moist carbon will tend to cake on the side of the grinder, and will feel moist. If the carbon is moist, dry it before use by heating in an oven or microwave. Take precautions handling the heated carbon to avoid burns. Allow the carbon to cool before grinding or combining with other ingredients. Store any unused dried carbon in an airtight container.

4) Grind the mixture to a fine powder. It is important that we grind the mixture as fine and uniformly as possible, about the consistency of coarse flour.

5) Sift the mixture into the beaker using a wire mesh strainer placed inside a large funnel to minimize dusting. When grinding and sifting, be careful with vents, fans and open windows, so your pseudo doesn't blow away as dust. You also don't want to inhale NaOH or carbon dust. Let the dust settle in the coffee grinder before opening the lid.

6) For every gram of total pill mass, add:
- 1.5 mL dry acetone

This measurement will get you in the ballpark. We want the mixture to be a liquid at this point, not a paste. Add more acetone in small increments, as the mixture will go from stiff to fluid very quickly. Acetone used for this purpose should be dried before use, as the moisture content of acetone can vary over such a wide range that the only way to obtain consistent results it to dry the acetone before use.

7) For every box of pills used add, while stirring:
- 3 drops distilled H2O (use the baby medicine dropper)

Why are we using dry acetone and then adding water? Since the amount of moisture present is critical for proper basing, and the water content of non-dried acetone is widely variable, the only way to accurately control the moisture available for basing is to dry the acetone first, then add a measured amount of water.

8) Stir with a glass rod for about 3 to 4 minutes. The mixture will slowly thicken to a wet paste.

9) For every box of pills used, add:
- 1.0 g corn starch

10) Stir for a few minutes. The mixture will become very stiff and the consistency of damp potting soil, with no signs of visible liquid. Add more cornstarch in very small increments if necessary.

Why the cornstarch? The cornstarch is a great absorbent and helps to dry our mixture fast. When drying the cornstarch will keep our mixture from turning into hard little rocks and when powdered again keeps the mixture free flowing. It also will help absorb waxy gak when we extract our free base.

11) Spread out the mixture on the pie plate(s) and let dry completely. It will dry fast because the carbon has increased the surface area of our mixture.

12) When completely dry sift the mixture back into the beaker using the wire mesh strainer placed inside a large funnel.

13) For every box of pills used, add:
- 35 mL Naphtha

14) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a few minutes.

Isn't boiling naphtha dangerous? Boiling any flammable solvent is an extremely dangerous practice. Solvents should not be heated over an open flame or on any apparatus that is capable of producing a spark. This includes defective or damaged electric hot plates. Adequate ventilation is required. This should not be done in a closed environment due to risk of explosion and/or fire and due to health concerns regarding inhalation of solvent fumes. The constant use of a fan positioned to blow across the solvent will disburse the vapor, reduce the risk of fire and explosion.

15) While waiting, make a Charmin filter. Take 4 plys of Charmin and fold three times to make a square. Fold that over once and then once again to make a quarter square. Completely wet the square with some clean naphtha using the medicine dropper and place the pad into the bottom of the funnel across the neck. The Charmin should not be "packed" or "compressed". Gently mold the edges around the contour of the funnel bottom. Wet it again with naphtha and place this filter-funnel into the Erlenmeyer flask.

16) Slowly decant the naphtha into the funnel in small amounts and allow it to filter through the Charmin into the flask. Don't pour in more than can pass through the Charmin in more or less real time. If you make a big puddle it may start to crystallize in the funnel, clogging the filter. The filtered naphtha should be crystal clear. Free base crystals will start to form in the filtrate. Set the flask aside.

17) For every box of pills used, add:
- 20 mL Naphtha

18) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a minute.

19) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Don't pour in more than can pass through the Charmin in more or less real time. Do not replace the Charmin, continue to re-use the same pad.

20) For every box of pills used add:
- 10 mL Naphtha

21) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate.

22) Slowly decant the naphtha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask, combining filtrates. Then empty the entire contents of the beaker into the filter funnel and let drain.

23) While draining, boil a small amount of naphtha, about 5 mL for every box of pills used. When all the liquid appears to have drained through, pour the boiling naphtha over the filter cake and let it drain again. Then take a large spoon and press down on top of filter cake, squeezing any remaining naphtha into the flask.

Should I do a fourth pull? You can try but tests have shown it's usually not enough gain to justify the effort. Only do additional pulls if the end result is less than 45 %.

24) Place the Erlenmeyer flask with the combined filtrate on the hot plate set to med high. Heat to boiling or until all crystals have re-dissolved. Pour the hot filtrate into clean pie plate(s).

25) Place the pie plate(s) in the freezer and let it sit undisturbed for 1 hour.

26) Remove the pie plate(s) from the freezer and pour off the used naphtha, filtering out free base crystals using a coffee filter. Let the collected free base crystals dry. Some crystals may adhere to the pie plate. Let them dry before removing.

27) After filtering crystals out, return the used naphtha to the beaker. Return all filtered solids, including the Charmin filter, to the beaker. Break solids up with a glass rod and mix well. Return to hot plate on med high heat. With constant gentle stirring, bring the used mixture back to boiling. Let boil for 1 minute. Turn heat off but leave beaker on hot plate. Make a new Charmin filter as per previous step 15. Filter liquid first, then add remaining solids to funnel to drain. Then take a large spoon and press down on top of rhe filter cake, squeezing any remaining naphtha into the flask. Place into freezer again for at least 30 minutes. You can assemble a few extra percent. It helped recover one botched batch that would've been poor otherwise.

28) The remaining naphtha does contain some additional pseudoephedrine free base. You may wash the naphtha thoroughly with warm distilled water and titrate to obtain the remaining pseudoephedrine in HCL form. This pseudoephedrine HCL will not be as clean as the free base, and will need to be rinsed with acetone, then recrystallized twice before being added to a reaction. The use of this pseudoephedrine with the free base is not recommended. This pseudoephedrine HCl can be accumulated until the quantity is sufficient to react by itself.

29) If the HCl salt is the desired outcome, redissolve the free base crystals in to a nonpolar and gas accordingly. Do Not gas the original Naphtha. If you gas the original naphtha, you will pick up unwanted contaminants. You may alternatively move the free base crystals into a small quantity of distilled H2O, and add HCl drop wise with stirring until the free base crystals all dissolve. Evaporate over low heat until this alligators over, then flash with dry acetone. Filter the acetone and pseudoehphedrine HCl through a coffee filter, rinse with acetone, allow drying.

Calculating Yield

When calculating your yield, remember to adjust for free base. Pseudo HCl is about 202 g per mole and pseudo free base is about 166 g per mole. So 166 divided by 202 is a ratio of 0.82 So, potential yield from 1 box of 120's would be 20 x 120 x 0.82 = 1.9 g free base vs 2.4 g for pseudo HCl.

Advantages and Disadvantages

The technique should be, in the near future, virtually universal. It should successfully extract most pseudoephedrine pills. The materials are easily available and draw less attention than xylene and tolulene purchases. Yields should range in the sixty percent range. The pseudoephedrine so obtained will be very clean-characteristic of A/B extractions of pseudoephedrine. The main disadvantage is heating a flammable solvent.

Time

You can run it in about 3 hours start to finish, 4 hours with the fourth pull. The first few times I would allow 5 hours to be safe until you get the feel of it. Each box of pills used has the potential of 1.9 g of free base. This is equivalent to 2.4 g of the HCL salt.
The average chemist with fair lab skills should be able to consistently achieve 1 gram of super clean free base per box, or 52%.
The experienced chemist with good lab skills should be able to consistently achieve 1.2 g of super clean free base per box or 63 - 65% seems to be the wall in its current form, but we're working on a few solutions.

Crystallization can take two different forms
The fast way: Placing the hot naphtha immediately in the freezer with no cool down will generally produce fine snow like crystals.
If you're not in a hurry: let the naphtha cool to about room temperature before placing into the freezer, and you will generally get large sparkling beauties like these.


Method 2

Summary

A new twist for producing clean pseudo HCl in high yields from an ever-changing array of pills. It's not only water less like in method above, it's simpler with no A/B at all. It's Method 2 or straight to the extraction. It is a simple extraction method that will bypass most of today’s modern adulterants and will return a very high yield of clean pseudo HCl. This can then be recrystallized or turned into free base to produce a pristine product. This method was written to be easily scalable and is very over the counter. Average yields have been 80 % to 90 % of clean pseudo HCl.

Equipment and glassware:

  • Three beakers or other heatproof glassware containers (approximately 200ml for every box of pills used)
  • One elemeyer flask or other heatproof glassware container (approximately 200ml for every box of pills used)
  • One graduated cylinder 100 -200 mL or other liquid measuring device in mLs
  • Two 5" glass funnels or plastic fuel funnels
  • Filter Paper or coffee filters
  • Glass stirring rod or bamboo skewers
  • Hot plate
  • Small fan
  • Small-scale weighing in grams
  • Safety glasses, latex gloves
  • Thermometer that is scaled to at least 120°C

Reagents:

  • 91- 99% Isopropyl Alcohol (drug store)
  • MEK Methyl Ethyl Ketone (paint / hardware store)
  • VM&P Naphtha - no substitutions (paint / hardware store)
  • (Do Not use Colemans, pet ether, lighter fluid, etc.)
  • Xylene (paint / hardware store)

Drying Aids:

  • Oven dried Epsom Salts or Washing Soda (drug / food store)
  • Salt (food store)

Abstract of Procedure

  1. Make extraction fluid.
  2. Place whole pills into beaker.
  3. Add extraction fluid.
  4. Heat to boiling, stirring until pills dissolve.
  5. Filter while hot into elemeyer flask.
  6. Repeat two times.
  7. Return combined extractions to clean beaker.
  8. Add Xylene
  9. Heat to 105 °C to boil off alcohol.
  10. Filter out pseudo HCl.
  11. Wash pseudo HCl with MEK and let dry.

Procedure
1) For every box of pills used: combine the following solvents and drying materials in a clean beaker and in the following order:
70 mL Isopropyl Alcohol
70 mL VM&P Naphtha
2 g of salt
4 g of dried epsom salts or dried washing soda


2) Stir with a glass rod for a few minutes, then let settle for 10 minutes. Depending on how much water was in the isopropyl alcohol to start with, the mixture will settle into 2 layers or 1 layer with damp solids at the bottom.

Why not use pre dried solvents to begin with? - that is perfectly ok if you have them, but I have noticed that adding the isopropyl and naphtha together almost always releases some water, no matter how dry they were ahead of time, so I would not skip this step.

3) Filter this into the elemeyer flask leaving any solids or bottom liquid layer behind and then transfer this solution into the second clean beaker.

4) Place whole pills in the third clean beaker.

Why whole pills? Don’t I need to grind them up first? - no, we are trying to keep loss to a minimum and grinding is not necessary as the isopropyl / naphtha mixture will dissolve them very well.

5) Pour 1/3 solvent mixture over pills.

6) Place the beaker on the hotplate and bring to a boil using medium hi heat. Use the small fan to keep vapors from accumulating. Stir occasionally with a glass rod until pills have dissolved into powder. Let boil for 1-2 minutes.

7) Place a funnel with filter paper in the elemeyer flask. Filter the solvent mixture while hot, leaving as much of the solids in the beaker as possible.

8) Return any solids to the beaker and repeat steps 5 through 7 two times, combining the extractions in the elemeyer flask.

9) For every box of pills used, add to the combined extractions:
- 50 mL Xylene

10) Transfer the extraction mixture back to the empty solvent beaker and place the beaker on the hotplate. Bring to a boil using the small fan to keep vapors from accumulating. Boil until the solution reaches 105 °C.

11) Using a clean funnel and filter, paper filter off the pseudo HCl while the solution is hot.

12) Rinse the pseudo HCl with a generous amount of MEK while in the funnel.

13) Remove filter and filter cake from funnel and allow to dry completely. (no more MEK smell)

14) Weight and enjoy, yield should be between 80 % to 90 % Introduction
G.Patton
 

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bigbadbear

Don't buy from me
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I think it's possible
G.Pattonthank you for your time brother I am coming back from the pharmacy now. They said that you must have a prescription from a specialist doctor to buy it. Only two glasses can be bought😐😐😑😑
I have to find another way

see you next time
 

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