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1-Phenyl-2-propanone (P2P) Leuckart amination to amphetamine and methamphetamine. Smale scale.

William D.

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Amphetamine
Reagents:
  • 1-Phenyl-2-propanone (P2P) 0.827 g, 6.2 mmol;
  • Formamide 3.5 ml;
  • Hydrogen peroxide (H2O2) 5 ml 30%;
  • Benzene 50 ml;
  • Magnesium sulphate (MgSO4);
  • Methanol 5 ml (MeOH);
  • Hydrochloric acid (15 % aq HCl) 5 ml;
  • Distilled water 25 ml;
  • Dichloromethane (DCM) 90 ml;
  • Sodium hydroxide (NaOH) pellets;
  • Sulfuric acid;
  • Acetone;
Equipment and glassware:
  • Pear shaped flask 10 ml;
  • Heating plate;
  • Boiling chips;
  • Funnel;
  • Rotary evaporator (optional);
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (50 mL x2, 100 mL x2);
  • Separatory funnel 100 ml;
  • Laboratory scale (0.1-200 g is suitable);
  • Measuring cylinders 10 mL and 100 mL;
  • Glass rod and spatula;
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
YrE8sW0dQo
1. A mixture of 1-phenyl-2-propanone (P2P) 0.827 g, 6.2 mmol and formamide 3.5 ml is heated at 160-170 ℃ for 16 h in a 10 ml pear shaped flask with a reflux condenser.
2. The mixture is cooled to room temperature, hydrogen peroxide 5 ml 30% (H2O2) is added. The mixture is stirred for 15 min.
3. The reaction mixture is
extracted with benzene (2x25 ml) is separatory funnel. Extract is dried over magnesium sulphate (MgSO4) and filtered. A dark oil is obtained after benzene evaporation from combined extract.
4. The dark oil is dissolved in a mixture of methanol 5 ml (MeOH) and hydrochloric acid (15% HCl) 5 ml and refluxed with a constant stirring for 2 h.
5. The reaction mixture is evaporated under reduced pressure. Next, the remaining product is dissolved in distilled water 25 ml and extracted with dichloromethane (DCM) CH2Cl2 (2x20 ml).
6. The aqueous solution is alkalized to pH 10 by addition sodium hydroxide (NaOH) pellets and extracted with DCM (2x25 ml).
7. The combined DCM extracts are evaporated. The amphetamine free base is obtained as a yellow oil.
8. Amphetamine sulphate
is prepared by addition of sulfuric acid in dry acetone in a volume ratio of 1:10 to pH 6. Product is filtered on Buchner flask and funnel, washed with a small amount of dry cold acetone and air dried (better to use vacuum desiccator to increase drying speed).


Methamphetamine
Download Video
Reagents:
  • 1-Phenyl-2-propanone (P2P) 5.4 mL, 40.2 mmol;
  • N-methylformamide 13.4 mL, 229 mmol;
  • Magnesium sulphate (MgSO4);
  • Hydrochloric acid (36-37% aq HCl) 10.7 mL, 0.004 mmol;
  • Toluene 60 ml;
  • Sodium hydroxide (NaOH);
  • Distilled water;
  • Acetone;
  • Hydrogen chloride gas (HCl);
Equipment and glassware:
  • Pear shaped flask 50 ml;
  • Heating plate;
  • Boiling chips;
  • Funnel;
  • Rotary evaporator (optional);
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (50 mL x2, 100 mL x2);
  • Separatory funnel 100 ml;
  • Laboratory scale (0.1-200 g is suitable);
  • Measuring cylinders 10 mL and 100 mL;
  • Glass rod and spatula;
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
J2stEP04YF
1. N-methylformamide 13.4 mL, 229 mmol, 5.7 equiv is added to 1-phenyl-2-propanone (P2P) 5.4 mL, 40.2 mmol with a constant stirring in 50 ml pear shaped flask with a reflux condenser.
2. Reaction temperature is gradually increased to 165-170 °C and maintained for 24-36 h.
3. The reaction mixture is cooled to room temperature. Sodium hydroxide (10 M NaOH aq) solution 24 mL, 0.24 mmol is added and the reaction mixture is refluxed for 2 h.
4. The reaction mixture is cooled to room temperature and separated to different layers. An aqueous layer is discarded. Hydrochloric acid (36-37% aq HCl) 10.7 mL, 0.004 mmol is added to a red organic layer.
5. The organic mixture is
refluxed for 2 h. Then, the solution is cooled to room temperature. Sodium hydroxide (8.3 M aq NaOH) solution 16.0mL, 0.13 mmol is slowly added. The crude methamphetamine free base is extracted with toluene (3 × 20 mL).
6. Combined organic layers are
dried over MgSO4 and solvent is evaporated in vacuum. Crude methamphetamine free base is obtained as a brown oil.
7. Crude methamphetamine free base is distilled under vacuum (2 mbar, 60-100 °C) with help of Kugelrohr distillation apparatus (optional) to yield methamphetamine as a clear to pale yellow oil (2.5 g, 42%).


Methamphetamine hydrochloride crystallization
1. Free base is dissolved in toluene 50 mL and anhydrous hydrogen chloride gas (HCl) is bubbled through the solution until a white precipitate formation is over (pH 6).
2. The resulting white precipitate is filtered with help of Buchner flask and funnel, washed with small amount of toluene and dried under vacuum to produce methamphetamine hydrochloride as a white salt 2.0 g, 27%.
 
Last edited by a moderator:

Botsauto-Dutchland

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134g/m p2p 45g/m forma so i calculated :100
1,34g 0,5g X22
I have 30 g p2p so X 22 and i got
30g p2p forma 11gx 5 i read the reaction ratio was best 1:5 and formic acid as catalyst

and next i use hcl to Hydrolise but i had just 50% yield but i had to much water in the ammonium formate /formamide i had produced.
now i heated the solution format/formamide to 175 so i hope this helps..

So what is the yield of this method ?
 

Botsauto-Dutchland

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134g/m p2p 45g/m forma so i calculated :100
1,34g 0,5g X22
I have 30 g p2p so X 22 and i got
30g p2p forma 11gx 5 i read the reaction ratio was best 1:5 and formic acid as catalyst

and next i use hcl to Hydrolise but i had just 50% yield but i had to much water in the ammonium formate /formamide i had produced.
now i heated the solution format/formamide to 175 so i hope this helps..

So what is the yield of this method ?
Botsauto-Dutchlandyield is higher make sure the p2p is purified and dried, if you mix the formamide and p2p it should mix no layers. and preparing formamide/formate heat it up to 180 Short and then lower it until 170 until no water/acid distils and the just wait a bit more. when stop heating put a cap on the glasware so its air tight.
this way i had from p2p oil to a- 100ml to around 70ml but after vacuum distilling so i wasted some a in the pump and in the start and end i had 60ml perfectly clear a oil.
i wish i could write how much powder i could get 10ml a to aphosfate and to sulfate.

if perfectly pure 10ml 9.4g d/l Amphetamine base is mixed with acid(sulfuric98) what should the powder has in weight, and what should be the excact weight in acid to reach ph?
now with not self made oil it is 1ml acid on 10 grams A oil 10 grams powder. reaction is smoking more when no alcohol used for mixing.
should it be cleaner without ether-acid base wash and perform a steam distil from a stainless steal container steamed true a cooler. ( if the oil contains no p2p) what impurity comes with it.
 

Selassi

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Swim got a question regarding a different variation on this method:

After the first step (boiling with formic and formamid), they now boil again the organic phase with water and NaOH instead of the reflux with HCl.

Can someone explain to me the metrics on this different second step to me? Swim has never done it this way but it seems to save a lot of time in contrast to the oldschool method with refluxing HCl.

What strength of caustic/water and how much is introduced to the reactor per L of product?
How long should swim boil this reactionmixture at what temp?
 

Curiousonion

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Why such a low yield for this, does anyone have a higher yield method for methamphetamine?
 

KornerStore

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Why such a low yield for this, does anyone have a higher yield method for methamphetamine?
CuriousonionNot an expert, but there are many higher yielding methods. Mercury amalgam or a borohydride reduction are the most common methods outside the leuckart.

The leuckart is just low yielding, nothing can be done.about that. But reagents are simple and cheap, the process is simple, and one can also substitute n methyl formamide with formic acid and methylamine. So it has some pros and cons.
 

workworkwork

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Yield for methamphetamine is 27% and for amphetamine?

Some studies got good yields for Leuckart route,
like in this thread http://bbzzzsvqcrqtki6umym6itiixfhn...-bmk-5449-12-7-to-free-base-a-oil.2906/page-4
1) Take a 2L round-bottomed flask and add 433g of formic acid. Add slowly and in small quantities the 360g of ammonium carbonate. Wait between additions until the effervescence of CO2 stops. If this is not respected, there is a risk of overflowing.
2) Added to the prepared solution the 100mL of P2P.
3) Connected in reflux under good agitation.
4) Maintain a temperature of 160-165°C for 24 hours. You can do it in several 6-hour sessions, for example.
N-Formylamphetamine is the product with a yield up to 78%.

Im curious about this route because possible make in medium or big scale and precursors are very cheap.
 

Saul

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Yield for methamphetamine is 27% and for amphetamine?

Some studies got good yields for Eckhart route,
like in this thread http://bbzzzsvqcrqtki6umym6itiixfhn...-bmk-5449-12-7-to-free-base-a-oil.2906/page-4
1) Take a 2L round-bottomed flask and add 433g of formic acid. Add slowly and in small quantities the 360g of ammonium carbonate. Wait between additions until the effervescence of CO2 stops. If this is not respected, there is a risk of overflowing.
2) Added to the prepared solution to 100mL of P2P.
3) Connected in reflux under good agitation.
4) Maintain a temperature of 160-165°C for 24 hours. You can do it in several 6-hour sessions, for example.
N-Formylamphetamine is the product with a yield up to 78%.

I'm curious about this route because possible make in medium or big scale and precursors are very cheap.
workworkwork
that is not right wrong info that thesis guy make big mistakes

ammonium carbonate is never used directly with p2p.
First, ammonium formate is made.
The ammonium format is easily made via ammonium carbonate and formic acid. Titrate
to a nice pH of 7 and remove the water.
Only then can it be used with p2p
 

Saul

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So I now reach again the point where HCI comes in the game.
yesterday, my p2p boild 14 hours with ammonium format ph7
it looks , very good

I hate HCI
I can not stand it, don't know what it is but I dont wanna use it anymore .
this shit killing me and all my electric stuff to .

is there no other way for this last step ?
 

G.Patton

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I hate HCI
I can not stand it, don't know what it is but I dont wanna use it anymore .
this shit killing me and all my electric stuff to .
SaulDo you use reflux condenser and fume hood?
 

Saul

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Sonnettales

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yes I do but I can stand it only with HCI I have this problem
T0Runfortunately if they say gas it, youre gonna have to gas something. I have been gassing dioxane in advance so i have it on hand. i end up only having to do it 1-2 times a month. 99% isopropyl can also be used
 

Bartholomeus

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Does anyone have some real success stories on BIG scale with this Leuckart reaction when using p2p/formamide/formic acid to form a-oil?
Can someone with real life experience post his results, as this is really frustrating.
There are a lot of big labs in holland pumping out a-oil and somebody must really know the process
So please anyone who reads this and knows something please post your experiences
 

Saul

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Does anyone have some real success stories on BIG scale with this Leuckart reaction when using p2p/formamide/formic acid to form a-oil?
Can someone with real life experience post his results, as this is really frustrating.
There are a lot of big labs in holland pumping out a-oil and somebody must really know the process
So please anyone who reads this and knows something please post your experiences
ChingShih
they dont share it my friend only talks like they run the biggest lab in history
iam waithing 3 monts for the last step in this synthese.
 

sponsor

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134g/m p2p 45g/m forma so i calculated :100
1,34g 0,5g X22
I have 30 g p2p so X 22 and i got
30g p2p forma 11gx 5 i read the reaction ratio was best 1:5 and formic acid as catalyst

and next i use hcl to Hydrolise but i had just 50% yield but i had to much water in the ammonium formate /formamide i had produced.
now i heated the solution format/formamide to 175 so i hope this helps..

So what is the yield of this method ?
Dutch046
are you still active here sir ?
 

ossi

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Amphetamine
Reagents:
  • 1-Phenyl-2-propanone (P2P) 0.827 g, 6.2 mmol;
  • Formamide 3.5 ml;
  • Hydrogen peroxide (H2O2) 5 ml 30%;
  • Benzene 50 ml;
  • Magnesium sulphate (MgSO4);
  • Methanol 5 ml (MeOH);
  • Hydrochloric acid (15 % aq HCl) 5 ml;
  • Distilled water 25 ml;
  • Dichloromethane (DCM) 90 ml;
  • Sodium hydroxide (NaOH) pellets;
  • Sulfuric acid;
  • Acetone;
Equipment and glassware:
  • Pear shaped flask 10 ml;
  • Heating plate;
  • Boiling chips;
  • Funnel;
  • Rotary evaporator (optional);
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (50 mL x2, 100 mL x2);
  • Separatory funnel 100 ml;
  • Laboratory scale (0.1-200 g is suitable);
  • Measuring cylinders 10 mL and 100 mL;
  • Glass rod and spatula;
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
1. A mixture of 1-phenyl-2-propanone (P2P) 0.827 g, 6.2 mmol and formamide 3.5 ml is heated at 160-170 ℃ for 16 h in a 10 ml pear shaped flask with a reflux condenser.
2. The mixture is cooled to room temperature, hydrogen peroxide 5 ml 30% (H2O2) is added. The mixture is stirred for 15 min.
3. The reaction mixture is
extracted with benzene (2x25 ml) is separatory funnel. Extract is dried over magnesium sulphate (MgSO4) and filtered. A dark oil is obtained after benzene evaporation from combined extract.
4. The dark oil is dissolved in a mixture of methanol 5 ml (MeOH) and hydrochloric acid (15% HCl) 5 ml and refluxed with a constant stirring for 2 h.
5. The reaction mixture is evaporated under reduced pressure. Next, the remaining product is dissolved in distilled water 25 ml and extracted with dichloromethane (DCM) CH2Cl2 (2x20 ml).
6. The aqueous solution is alkalized to pH 10 by addition sodium hydroxide (NaOH) pellets and extracted with DCM (2x25 ml).
7. The combined DCM extracts are evaporated. The amphetamine free base is obtained as a yellow oil.
8. Amphetamine sulphate
is prepared by addition of sulfuric acid in dry acetone in a volume ratio of 1:10 to pH 6. Product is filtered on Buchner flask and funnel, washed with a small amount of dry cold acetone and air dried (better to use vacuum desiccator to increase drying speed).


Methamphetamine
Reagents:
  • 1-Phenyl-2-propanone (P2P) 5.4 mL, 40.2 mmol;
  • N-methylformamide 13.4 mL, 229 mmol;
  • Magnesium sulphate (MgSO4);
  • Hydrochloric acid (36-37% aq HCl) 10.7 mL, 0.004 mmol;
  • Toluene 60 ml;
  • Sodium hydroxide (NaOH);
  • Distilled water;
  • Acetone;
  • Hydrogen chloride gas (HCl);
Equipment and glassware:
  • Pear shaped flask 50 ml;
  • Heating plate;
  • Boiling chips;
  • Funnel;
  • Rotary evaporator (optional);
  • Syringe or Pasteur pipette;
  • pH indicator papers;
  • Beakers (50 mL x2, 100 mL x2);
  • Separatory funnel 100 ml;
  • Laboratory scale (0.1-200 g is suitable);
  • Measuring cylinders 10 mL and 100 mL;
  • Glass rod and spatula;
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Filter paper;
1. N-methylformamide 13.4 mL, 229 mmol, 5.7 equiv is added to 1-phenyl-2-propanone (P2P) 5.4 mL, 40.2 mmol with a constant stirring in 50 ml pear shaped flask with a reflux condenser.
2. Reaction temperature is gradually increased to 165-170 °C and maintained for 24-36 h.
3. The reaction mixture is cooled to room temperature. Sodium hydroxide (10 M NaOH aq) solution 24 mL, 0.24 mmol is added and the reaction mixture is refluxed for 2 h.
4. The reaction mixture is cooled to room temperature and separated to different layers. An aqueous layer is discarded. Hydrochloric acid (36-37% aq HCl) 10.7 mL, 0.004 mmol is added to a red organic layer.
5. The organic mixture is
refluxed for 2 h. Then, the solution is cooled to room temperature. Sodium hydroxide (8.3 M aq NaOH) solution 16.0mL, 0.13 mmol is slowly added. The crude methamphetamine free base is extracted with toluene (3 × 20 mL).
6. Combined organic layers are
dried over MgSO4 and solvent is evaporated in vacuum. Crude methamphetamine free base is obtained as a brown oil.
7. Crude methamphetamine free base is distilled under vacuum (2 mbar, 60-100 °C) with help of Kugelrohr distillation apparatus (optional) to yield methamphetamine as a clear to pale yellow oil (2.5 g, 42%).


Methamphetamine hydrochloride crystallization
1. Free base is dissolved in toluene 50 mL and anhydrous hydrogen chloride gas (HCl) is bubbled through the solution until a white precipitate formation is over (pH 6).
2. The resulting white precipitate is filtered with help of Buchner flask and funnel, washed with small amount of toluene and dried under vacuum to produce methamphetamine hydrochloride as a white salt 2.0 g, 27%.
William Dampierhello,

that mean i need for 1000g P2P more than 50 liters Benzene and more than 90 liters DCM?
or do you need less for large quantities?

thx
 

Hank Schrader

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Many years ago, I worked with the Leuckart reaction. I have deduced the ideal proportions for obtaining the formyl derivative and the final hydrolysis of the product. I can only say that for the activation of the reaction, it is necessary to take a formic acid catalyst. I raise the temperature very slowly using an accurate temperature controller to slowly drive the water away. After 48 hours+, my formyl derivative yield is almost 95%+
Formyl derivative must be washed ideally with water!

The main losses in the reaction are usually associated with hydrolysis. Acid hydrolysis gives a yield of no more than 30-50% for amines. There are better methods of hydrolysis. Hydrolysis must be carried out in methanol and in the presence of KOH or NaOH.
 

Hank Schrader

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I also want to please you, a leukart can be made in a matter of minutes, it is enough to purchase a special chemical microwave and irradiate the mixture of formamide ketone and catalyst in stages.
The yield of formyl derivative is more than 95%.
This is a very good and repeatedly studied technology.

In the right hands, this knowledge will give you a great way out.
If you do the hydrolysis correctly, you will get a yield of over 90%!!!
In the hands of a person who knows what he is doing from 1 kg of unsubstituted ketone, 810-830 ML of the free base of the amine, purified by vacuum fractional distillation, is obtained. After neutralization (6.5-7 pH) and filtering on a centrifuge, we obtain a product that is filled with anhydrous acetone and mixed into a homogeneous mass and filtered again on a centrifuge. Getting 1020 - 1045g of snow-white amphetamine sulfate without a single smell of amine.
AEnjrhBxKk
 
Last edited:

OrgUnikum

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I also want to please you, a leukart can be made in a matter of minutes, it is enough to purchase a special chemical microwave and irradiate the mixture of formamide ketone and catalyst in stages.
The yield of formyl derivative is more than 95%.
This is a very good and repeatedly studied technology.

In the right hands, this knowledge will give you a great way out.
If you do the hydrolysis correctly, you will get a yield of over 90%!!!
In the hands of a person who knows what he is doing from 1 kg of unsubstituted ketone, 810-830 ML of the free base of the amine, purified by vacuum fractional distillation, is obtained. After neutralization (6.5-7 pH) and filtering on a centrifuge, we obtain a product that is filled with anhydrous acetone and mixed into a homogeneous mass and filtered again on a centrifuge. Getting 1020 - 1045g of snow-white amphetamine sulfate without a single smell of amine. View attachment 7996
Hank SchraderRealworld working modified microwaves exist!
 

Attachments

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Hank Schrader

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I will share the table with you.
Khi3lZJupI
 

OrgUnikum

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Hank SchraderMaybe it is just fair to add that temperatures over 180 °C like the named 200 and 210 °C for sure completely destroy P2P and even the Formamide, the resulting vapors and gases are highly toxic. Vent everything coming from top of the condenser outsides! Seriously!
Keep it below 180, better below 175°C and calibrate the Infrared thermometer to the flask/setting you use or you will never exactly know how hot it is.

Good luck
 
View previous replies…

Throw-off

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When you say yields are not stellar what type of percentage are we talking? Is it not similar too the study above with the Methly derivative of formamide?

The reason for the use of D-(-)-Tartaric instead of the natural derived one is because I have it readily available and free. The solid mass is the D isomer and the solution is the L isomer correct?
Throw-offNever mind about the Tartaric question, I worked it out today. Thanks friend.
 

Throw-off

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Maybe it is just fair to add that temperatures over 180 °C like the named 200 and 210 °C for sure completely destroy P2P and even the Formamide, the resulting vapors and gases are highly toxic. Vent everything coming from top of the condenser outsides! Seriously!
Keep it below 180, better below 175°C and calibrate the Infrared thermometer to the flask/setting you use or you will never exactly know how hot it is.

Good luck
OrgUnikumWith Hydrolysis of the formyl amide in these measurements.
NMF - 130ml
P2P - 100ml
Formic - 84ml
How much naoh solution do you need and how much HCI? Is 35% lab grade sufficient?
 

OrgUnikum

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View previous replies…

Bartholomeus

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Many years ago, I worked with the Leuckart reaction. I have deduced the ideal proportions for obtaining the formyl derivative and the final hydrolysis of the product. I can only say that for the activation of the reaction, it is necessary to take a formic acid catalyst. I raise the temperature very slowly using an accurate temperature controller to slowly drive the water away. After 48 hours+, my formyl derivative yield is almost 95%+
Formyl derivative must be washed ideally with water!

The main losses in the reaction are usually associated with hydrolysis. Acid hydrolysis gives a yield of no more than 30-50% for amines. There are better methods of hydrolysis. Hydrolysis must be carried out in methanol and in the presence of KOH or NaOH.
Hank Schrader
Please check your PM
 

jokerr

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masters ;

@Hank Schrader can you synthesize an amphetamine by the method you mentioned?
Or can you open a topic and explain this synthesis to us in detail?
We will be very helpful for beginners.

p2p - amphetamine 90% efficiency is a very good figure.

@G.Patton
Could you please make a detailed subject or video of this synthesis?
 
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