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

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
 

Hank Schrader

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I will share the table with you.
Khi3lZJupI
 

OrgUnikum

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BamBam

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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%).

What’s other option? Simple, fractional or steam distillation? If don’t have Kugelrohr distillation apparatus?
 

rothschild33

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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%).

What’s other option? Simple, fractional or steam distillation? If don’t have Kugelrohr distillation apparatus?
BamBamWhat is the function of the NaOH in steam distillation?
 

btcboss2022

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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
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;
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 DampierRecently I started to alternate Leuckart route and NaBH4 route for D-Meth and
I had twice a strange situation in the Leuckart route.
After tartaric isomer separation when I turns the solid part alkali to remake separation the freebase goes to the bottom layer.
It only happened with the L-meth freebase from Leuckart route, before separation when its racemic in alkali ambient is top layer, the líquid part after isomer separation(D-meth freebase) when its alkali is top layer too as it should be but Lmeth freebase no.
Is strange and I dont have the explanation I dont know if someone has the same situation or know why this happens.
Thanks.
 

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w2x3f5

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Recently I started to alternate Leuckart route and NaBH4 route for D-Meth and
I had twice a strange situation in the Leuckart route.
After tartaric isomer separation when I turns the solid part alkali to remake separation the freebase goes to the bottom layer.
It only happened with the L-meth freebase from Leuckart route, before separation when its racemic in alkali ambient is top layer, the líquid part after isomer separation(D-meth freebase) when its alkali is top layer too as it should be but Lmeth freebase no.
Is strange and I dont have the explanation I dont know if someone has the same situation or know why this happens.
Thanks.
btcboss2022Even the color in the first photo says that you have dirty oil with a significant impurity, did you distill the amine after Leuckart-Wallach? Leuckart is known to give a mixture of various secondary/tertiary amines, possibly some other impurities. Hank Schrader posted an excerpt from the study, in which the formation of impurities in the Leuckart-Wallach reaction is considered in more detail.
Also, the separation of isomers could not have been satisfactory due to the low purity of the free base of the amine.
 
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btcboss2022

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the crystal can also be obtained from mix D and L isomers meth, I personally did it. You did not measure the angle of rotation.
w2x3f5No, I didnt distill it before isomer separation.
I dont have any problem with the separation process just was strange to find an impurity only when I wash the L freebase from Leuckart route.
I left steam distillation long time ago for large amounts, is a nightmare and eternal even with a big steamer.
I have exactly the same final stuff with acid base washing and recrystallization after acetone crystallization.
I know what theory and literature say about it but its a fact proved myself hundreds of times.
About rotation angle you are right I didnt check it but my customers and some of them are old meth users tell me how powerfull is and racemic one is not as powerfull as this one.
This pic is about a small batch crystallization for some small orders but now Im working in a big batch and I will show you how transparent and big could be the shards.
I would be very grateful if you explain me how you obtain big and transparent crystals from racemic freebase I read that something like medium ones are possible but honestly I never seen it.
I'm thinking in propose you a little challenge and tell me what you think.
I can send you a sample of my D-meth and a sample of my racemic MDMA.
You make all the tests that you need, take them to a trusted lab, give them to experienced users...what you want.
With the results in hand if you can prove me that your stuff from distilled freebase is more pure or better than mine from not distill it I send you 250gr of each product for free if you cant I only want that you say that you were wrong here in forum.
I think its a good deal no?
What you think?
Thanks.
 

btcboss2022

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No, I didnt distill it before isomer separation.
I dont have any problem with the separation process just was strange to find an impurity only when I wash the L freebase from Leuckart route.
I left steam distillation long time ago for large amounts, is a nightmare and eternal even with a big steamer.
I have exactly the same final stuff with acid base washing and recrystallization after acetone crystallization.
I know what theory and literature say about it but its a fact proved myself hundreds of times.
About rotation angle you are right I didnt check it but my customers and some of them are old meth users tell me how powerfull is and racemic one is not as powerfull as this one.
This pic is about a small batch crystallization for some small orders but now Im working in a big batch and I will show you how transparent and big could be the shards.
I would be very grateful if you explain me how you obtain big and transparent crystals from racemic freebase I read that something like medium ones are possible but honestly I never seen it.
I'm thinking in propose you a little challenge and tell me what you think.
I can send you a sample of my D-meth and a sample of my racemic MDMA.
You make all the tests that you need, take them to a trusted lab, give them to experienced users...what you want.
With the results in hand if you can prove me that your stuff from distilled freebase is more pure or better than mine from not distill it I send you 250gr of each product for free if you cant I only want that you say that you were wrong here in forum.
I think its a good deal no?
What you think?
Thanks.
btcboss2022I know it sounds greedy from my side but I just want to demonstrate that at least in Meth and MDMA steam distillation could be avoided and have the purest product anyway.
I found the way after many tests because steam distillation was a terrible nightmare for my mind trust me.
 

w2x3f5

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I know it sounds greedy from my side but I just want to demonstrate that at least in Meth and MDMA steam distillation could be avoided and have the purest product anyway.
I found the way after many tests because steam distillation was a terrible nightmare for my mind trust me.
btcboss20221. Steam distillation will separate the amine mixture very poorly, vacuum distillation is the best solution and is quite fast in the presence of a strong vacuum.
2. I'm afraid to lie, but as far as I remember, after a single separation of isomers, the final composition of the "d-isomer of tartrate" is about 80-90 percent of the d isomer and the rest is the l isomer.
3. I made glass without separation of isomers from a mixture of alcohol and a small amount of water + additional components, I got a glass monolithic mass, cracks appeared when it dried completely, especially if the crystals were washed with acetone (do not repeat my mistake), but the mass remained transparent. In my case, I did not use glassware for crystallization and other nuances, I spent 2-3 months on the selection of a technique.
Before this method, I tried to make from a melt of salt, monolithic pieces were obtained, but not transparent, only blotches of transparent crystals. There was an idea to do something like zone melting.

Why do I need to prove something to you? I shared my experience, if you are not interested in it, this is your personal business. Do you really think that I need your 250 grams, it doesn’t matter to me at all, I won’t mess around with trifles. Consumers do not give an objective assessment of the purity of substances, it is enough to ask them what is better mephedrone powder or a large crystal, guess what they will answer ... Half of the effect of drugs (stimulants for sure) is their appearance)))

I almost forgot, if you plan to distill in a vacuum, then you definitely need an along spider, since there will be light-boiling fractions of garbage, with the help of a spider you can change the receiving flask without stopping the distillation of the amine, similar to a revolver, but instead of cartridges, flasks.
 

w2x3f5

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1. Steam distillation will separate the amine mixture very poorly, vacuum distillation is the best solution and is quite fast in the presence of a strong vacuum.
2. I'm afraid to lie, but as far as I remember, after a single separation of isomers, the final composition of the "d-isomer of tartrate" is about 80-90 percent of the d isomer and the rest is the l isomer.
3. I made glass without separation of isomers from a mixture of alcohol and a small amount of water + additional components, I got a glass monolithic mass, cracks appeared when it dried completely, especially if the crystals were washed with acetone (do not repeat my mistake), but the mass remained transparent. In my case, I did not use glassware for crystallization and other nuances, I spent 2-3 months on the selection of a technique.
Before this method, I tried to make from a melt of salt, monolithic pieces were obtained, but not transparent, only blotches of transparent crystals. There was an idea to do something like zone melting.

Why do I need to prove something to you? I shared my experience, if you are not interested in it, this is your personal business. Do you really think that I need your 250 grams, it doesn’t matter to me at all, I won’t mess around with trifles. Consumers do not give an objective assessment of the purity of substances, it is enough to ask them what is better mephedrone powder or a large crystal, guess what they will answer ... Half of the effect of drugs (stimulants for sure) is their appearance)))

I almost forgot, if you plan to distill in a vacuum, then you definitely need an along spider, since there will be light-boiling fractions of garbage, with the help of a spider you can change the receiving flask without stopping the distillation of the amine, similar to a revolver, but instead of cartridges, flasks.
w2x3f5The main rule of the manufacturer, never take other people's drugs or the price will be too high.
 

btcboss2022

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1. Steam distillation will separate the amine mixture very poorly, vacuum distillation is the best solution and is quite fast in the presence of a strong vacuum.
2. I'm afraid to lie, but as far as I remember, after a single separation of isomers, the final composition of the "d-isomer of tartrate" is about 80-90 percent of the d isomer and the rest is the l isomer.
3. I made glass without separation of isomers from a mixture of alcohol and a small amount of water + additional components, I got a glass monolithic mass, cracks appeared when it dried completely, especially if the crystals were washed with acetone (do not repeat my mistake), but the mass remained transparent. In my case, I did not use glassware for crystallization and other nuances, I spent 2-3 months on the selection of a technique.
Before this method, I tried to make from a melt of salt, monolithic pieces were obtained, but not transparent, only blotches of transparent crystals. There was an idea to do something like zone melting.

Why do I need to prove something to you? I shared my experience, if you are not interested in it, this is your personal business. Do you really think that I need your 250 grams, it doesn’t matter to me at all, I won’t mess around with trifles. Consumers do not give an objective assessment of the purity of substances, it is enough to ask them what is better mephedrone powder or a large crystal, guess what they will answer ... Half of the effect of drugs (stimulants for sure) is their appearance)))

I almost forgot, if you plan to distill in a vacuum, then you definitely need an along spider, since there will be light-boiling fractions of garbage, with the help of a spider you can change the receiving flask without stopping the distillation of the amine, similar to a revolver, but instead of cartridges, flasks.
w2x3f5You are totally right was a stupid idea and I apologize about it Im really sorry.
About purity I have lab reports of 93 and 95% Im not based only in customers opinions.
About point 2 yes its correct is around this %
About point 3 I would be very interested in the detailed process you can PM if you prefer.
I cleaned a liter of meth freebase to show you how looks like after the cleaning process.
I made vacuum distillation in past and even more slow than steam :-(
Thanks and sorry again about yesterday message :-(
 

btcboss2022

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You are totally right was a stupid idea and I apologize about it Im really sorry.
About purity I have lab reports of 93 and 95% Im not based only in customers opinions.
About point 2 yes its correct is around this %
About point 3 I would be very interested in the detailed process you can PM if you prefer.
I cleaned a liter of meth freebase to show you how looks like after the cleaning process.
I made vacuum distillation in past and even more slow than steam :-(
Thanks and sorry again about yesterday message :-(
btcboss2022Pics
 

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w2x3f5

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You are totally right was a stupid idea and I apologize about it Im really sorry.
About purity I have lab reports of 93 and 95% Im not based only in customers opinions.
About point 2 yes its correct is around this %
About point 3 I would be very interested in the detailed process you can PM if you prefer.
I cleaned a liter of meth freebase to show you how looks like after the cleaning process.
I made vacuum distillation in past and even more slow than steam :-(
Thanks and sorry again about yesterday message :-(
btcboss2022I can send you in private messages a photo of glass obtained from dirty amine oil. I studied the possibility of obtaining large pieces of glass without vacuum distillation, also there was no separation into isomers.
 

btcboss2022

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it is an oil with impurities, distilled in fractions in a vacuum, a completely colorless oil, without yellow tints.
w2x3f5I know how pure meth freebase looks like I used to do steam distillation and did vacuum too you must think that freebase of the pic still needs to be extracted and dried but as I explained I'm able to obtain the exactly same pure and strong final product from this freebase, avoiding distillations, than from the distilled one, you won't distinguish them in fact nobody told me anything about any difference in the product and I changed the process long time ago without saying and lab reports indicate exactly the same purity %
Happy to receive the pics thanks.
 

MisterAnonymous

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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
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;
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 Dampier@[SIZE=17px]William Dampier[/SIZE]
Can you please be more detailed about step 8 of the Amphetamine synthese? Thanks in advance.
 

situ1984

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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
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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 DampierCan methamphetamine free base in the form of oil be directly changed to dextrorotation?
 

G.Patton

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Can methamphetamine free base in the form of oil be directly changed to dextrorotation?
situ1984Hello, as I know, there is just one way - conventional isomer separation with tartactic (or another carboxylic acid)
 
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