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Ephedrine extraction from pills methods

G.Patton

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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.
FoNuMbKrTw

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.
JDrHywY0A4


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
 
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ralralro

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I wonder that I need 100% xylene or is it okay to just use the paint shop xylene?
 

G.Patton

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I wonder that I need 100% xylene or is it okay to just use the paint shop xylene?
Hi. It depends on composition of paint shop xylene
 
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diogenes

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Hi, I have found an over the counter product containing Pseudo + Ibuprofen in a gel capsule. First it seemed easy to extract as the substances are already in solution, Ibuprofen is only soluble in water when basis, so the opposite of pseudo. When I looked at the detailed ingredients, however, it turned out that the liquid inside the capsule contains Macrogol 600, a form of PEG (Polyethyleneglycol), which seems to be a bitch to get rid of. The only idea I have now is that PEG is poorly soluble in ether, so I could add some ether to the liquid squeezed out of the capsules, then some KOH or NaOH so that the pseudo can walk over to the ether. As PEG is not completely insoluble in ether this would need to be repeated I guess.

My questions:
Do you think this would work? Or do you know a better method?

Would any of the above methods work and get rid of the PEG?

Thank you.
 

G.Patton

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Hi, I have found an over the counter product containing Pseudo + Ibuprofen in a gel capsule. First it seemed easy to extract as the substances are already in solution, Ibuprofen is only soluble in water when basis, so the opposite of pseudo. When I looked at the detailed ingredients, however, it turned out that the liquid inside the capsule contains Macrogol 600, a form of PEG (Polyethyleneglycol), which seems to be a bitch to get rid of. The only idea I have now is that PEG is poorly soluble in ether, so I could add some ether to the liquid squeezed out of the capsules, then some KOH or NaOH so that the pseudo can walk over to the ether. As PEG is not completely insoluble in ether this would need to be repeated I guess.

My questions:
Do you think this would work? Or do you know a better method?

Would any of the above methods work and get rid of the PEG?

Thank you.
Separating ibuprofen from pseudoephedrine should be fairly simple, as ibuprofen is a carboxylic acid whereas pseudoephedrine is an amine. The pseudoephedrine will be water-soluble in acidic water, while the ibuprofen will not. If the pka of ibuprofen is between 4-5, you'll want a rather acidic solution to convert most of it to its free acid form; a pH of 3 should do nicely. This low pH can be achieved easily with hydrochloric (muriatic acid). Polyethylene glycol is water-soluble polymer, you can extract pseudo from water with help of ether or petroleum ether.
 
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diogenes

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There is link above to an Erowid page where a water free extraction is described which can be used when a medication contains PEG. It recommends to start with a non-polar solvent such as Xylene or Toluene and soak the powder for at least 6 hours (for PEG), I guess in this time the PEG dissolves in the non-polar as well? My problem is that my starting capsule is filled with a liquid containing a slightly basic solution of PEG, water, KOH, Ibuprofen and Pseudo. I have added some toluene, and tried drying with some 3A molecular sieves, then added some diluted HCl to neutralise the KOH and make sure the pseudo is not in the Toluene layer which is meant to be discarded with the PEG dissolved.

When the HCl was added something precipitated this could have been the Ibuprofen. I removed the water layer and the precipitate. This is where I am at now. My concern is that with this method there could be some PEG in the water layer if PEG migrated due to its higher solubility in water.
 

G.Patton

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I guess in this time the PEG dissolves in the non-polar as well?
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.
 
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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.
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.
 

G.Patton

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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.
Yes, you are right.
 
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