G.Patton

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Introduction

Amphetamine can be obtained in a 30% yield in a one-step synthesis by refluxing phenylacetone in ethanol with ammonia, aluminium grit, and a small quantity of mercuric chloride. By trying out this reaction procedure for amphetamine, it was found that the yield of the reaction was not as high as for Pervitin (30% and 70%, respectively). However, the easiness of the procedure makes this method worthwhile. It's the simplest way to obtain amphetamine sulphate from P2P. Another way you can learn in Synthesis of Dextroamphetamine from P2P with (S)-(−)-α-Methylbenzylamine topic.

Equipment and glassware:

Reagents:

  • 40 g, 0.3 mole Phenylacetone (P2P) [CAS: 103-79-7];
  • 200 mL Ethanol (EtOH) 96-98 %
  • 200 mL 25 % Ammonia alc. (NH4OH);
  • 40 g, 1.5 moles Al-grit;
  • 0.3 g,1 mmol Mercury chloride (2) (HgCl2);
  • ~200 mL Distilled water;
  • 120 g Potassium hydroxide (KOH);
  • ~450 mL Diethyl ether (Et2O);
  • ~ 200 mL Hydrochloric acid 20 % (HCl) aq. solution;
  • ~ 200 g Sodium sulfate (Na2SO4);
  • ~30 mL Sulfuric acid conc. 98%.
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1-Phenyl-2-aminopropane sulfate:
Boiling Point (free base): 200-203 °C at 760 mm Hg;
Melting Point: 280-281 °C;
Molecular Weight: 368.5 g/mol;
Density: 0.936 g/mL;
CAS Number: 60-13-9.

Procedure

A mixture of 40 g (0.3 mole) phenylacetone, 200 mL ethanol, 200 mL 25 % ammonia, 40 g (1.5 mole) Al-grit and 0.3 g (1 mmol) HgCl2 is warmed with vigorous stirring in 2 L round bottom flask with reflux condenser until reaction takes place, after which warming is stopped immediately. Cooling should be applied if the reaction becomes too violent. When the violence of the reaction has diminished, the mixture is refluxed with vigorous stirring for about 2 h, concentrated in vacuo to 200 mL and poured into ice water, alkalinized with 120 g KOH, and extracted with ether (100 mL x 3). The extractions are treated with 20 % HCl, the resulting water layer alkalinized and extracted with 150 mL ether. The organic layer is dried over Na2SO4, the ether evaporated, and the residue distilled in vacuo. Yield: 12.5 g (30 %).
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Preparation of amphetamine sulfate by addition of sulfuric acid drop-wise is yielded 96-98 % product with a purity of 99.2-99.8 % (USP grade), which was filtered as white powder on the Buchner flask and funnel and air dried. Here and here you can find video and photo-manuals of acidifying procedures respectively.
 
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Mr.Blanks00

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hello sir, sorry i want to ask. I have made amphetamines in this way I get a layer of oil as much as 25 grams and when I make sulfate salt I get 8 grams, while from the solution I extract it and get only 1 gram, is this appropriate or not sir, sorry sir 1 more for how to use this amphetamine how many mg for the moderate dose and how do you use it, is it a pill or what, sir, please advise sir, thank you.
 

G.Patton

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hello sir, sorry i want to ask. I have made amphetamines in this way I get a layer of oil as much as 25 grams and when I make sulfate salt I get 8 grams, while from the solution I extract it and get only 1 gram, is this appropriate or not sir, sorry sir 1 more for how to use this amphetamine how many mg for the moderate dose and how do you use it, is it a pill or what, sir, please advise sir, thank you.
YusufHello, 9g in total is to small (~21% conversion). How much P2P have you used? Probably you got 25 g not pure amphetamine free base or I didn't understand your text clearly.
how to use this amphetamine how many mg for the moderate dose and how do you use it, is it a pill or what, sir, please advise sir, thank you.
You can open BB Wiki ==> Amphetamine and read about.
 

Mr.Blanks00

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I used 40gram p2p , I got 25gram free base oil, but when I made sulfate salt I only got 8gram.
 

G.Patton

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I used 40gram p2p , I got 25gram free base oil
YusufIt is quite good yield, 62.5%. I think there is not pure amphetamine free base. You can check boiling point of your oil. If it is very different from amphetamine, you can vacuum distill it.
 

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hello, i have freebase a-oil but i have some problems. it is crystal clear but the ph is 11.8. and it also smell like caustic. what should i do to purefy it. i have done normale distillation because i can reach high temperature. should i wash it with boiling water?
 

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studentt

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above 200c. i don’t know exactly because my heatingmantle is without display. but when i distilled it. reach the boiling ponit it was something like gas. and turn back to liquid.
 

G.Patton

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above 200c. i don’t know exactly because my heatingmantle is without display. but when i distilled it. reach the boiling ponit it was something like gas. and turn back to liquid.
studenttBoiling point is indirect confirmation of substance purity. You can read here to understand it clearly Boiling point determination. The thermometer must be used for distillation purposes.
 

Sweswe

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at what scale can this synthesis be done in? is there any other process when it comes to around 1l p2p
 

G.Patton

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at what scale can this synthesis be done in? is there any other process when it comes to around 1l p2p
SwesweI think reaction will be too violent and a yield will be decreased. I'm not sure that you can scale it more than 100g.
 

Sweswe

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I think reaction will be too violent and a yield will be decreased. I'm not sure that you can scale it more than 100g.
G.Pattonok thanks for reply! Do you know which route is best for larger batches? I've looked a bit at P2NP with NaBH4/CuCl2 (1kg scale) but I'm also looking for bigger than that if there's a possibility, sorry for asking here, know it doesn't belong in the thread

/Regards
 

Hank Schrader

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The yield can be increased up to 95%. The only condition is anhydrous ammonia.
 

Gale

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How much mercuric chloride you guys reccomend for 800g synth
 

Hank Schrader

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hello sir, how do you use anhydrous ammonia while the hgcl reaction must contain water content.. can you explain your method.
YusufIt's that simple. The technology has long been known, which uses an autoclave and anhydrous ammonia. The ammonia cylinder is connected to the autoclave and saturated with the icy methanol to the desired mass. Usually make a 10-12% solution of ammonia in methanol. Water will of course be in small quantities in the reaction because when imine is formed, the reaction releases water...
Amphetamine can be obtained both on aluminum and on other catalysts, but in the case of using Raney or other metals, hydrogen must be supplied to the reaction.
 

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hello sir, sorry i want to ask. I have made amphetamines in this way I get a layer of oil as much as 25 grams and when I make sulfate salt I get 8 grams, while from the solution I extract it and get only 1 gram, is this appropriate or not sir, sorry sir 1 more for how to use this amphetamine how many mg for the moderate dose and how do you use it, is it a pill or what, sir, please advise sir, thank you.
Yusufhello yusuf what is the latest status ? can you cook meth ?
 
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