Amphetamine Synthesis via P2P Oxime Reduction

GhostChemist

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Reactions proceed according to Scheme 1
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Reagents and Materials:

  • 8.1 g of aluminum
  • 0.05 g of mercury(II) chloride
  • 5 g P2P
  • 2 g of hydroxylamine or a mixture (50-60 ml of IPA (or ethanol) + 2.5 g of NaOH + 4.55 g of hydroxylamine hydrochloride)
  • 50 ml of ethanol
  • 2-liter flask
  • 2 liters of ice-cold water (500 g of ice)
  • 100 ml DCM
  • 10 ml of acetone
  • 1 ml of 89% sulfuric acid
  • pH indicator paper
  • Various-sized beakers
  • Heater

Synthesis Procedure

Starting materials for the synthesis. Fig 1
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In two separate beakers, hydroxylamine hydrochloride and sodium hydroxide are mixed with ethanol or IPA. Fig 2
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Next, the contents of the beakers are combined. Fig 3
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To the resulting mixture, P2P is added. The color changes from pale yellow to orange. Additionally, 50 ml of ethanol or IPA is added to the solution. Fig 4
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Next, aluminum amalgam is prepared using the standard method. Fig 5
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The prepared P2P oxime solution is added to the resulting aluminum amalgam, and a reflux condenser is connected. Fig 6
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The reaction proceeds slowly without significant heat generation, and additional cooling is not required. It is possible that with larger loads, the exothermic effect would be more pronounced. Fig 7
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The reaction is fully completed within 1-1.5 hours. Fig 8
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The reaction mass is filtered through a paper filter. Fig 9
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Due to the fine dispersion of the formed sediment, filtration is quite challenging. In this case, it is possible to perform the extraction of DСM from the reaction mixture directly with the sludge and then filter the organic extract. Fig 10
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The filtered DСM is dried with anhydrous sodium sulfate. Fig 11
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DCM is distilled off at a temperature of 90°C. Fig 12
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After distillation, a yellow-colored oil remains in the residue. Fig 13
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The obtained oil is transferred to a beaker, and any remaining residues in the flask are rinsed with acetone. The pH of the amphetamine oil is alkaline. Fig 14
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Sulfuric acid is added to the obtained amphetamine solution until the pH reaches 5-6, resulting in the precipitation of amphetamine sulfate. Fig 15
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The obtained solution is evaporated to half of its volume, and then 5 mL of anhydrous cold acetone is added. The precipitate is filtered off and dried. Fig 16
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The yield of amphetamine sulfate is 2.5 g, which corresponds to 36%.
 
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alterego

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Hi there, great write up!
So manny respect for u guys bringing this up/ take time to share with us!
But 1 thing strugles me.
This forum teached me that Amfetamine should be white, other colors are (faulty) synthesis related,precursor/ poison leftovers...
I know its common to have a slight color change in the end product, but your end product is just full yellow/orange color ?
Whats the deal about that ?
 

GhostChemist

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Hi there, great write up!
So manny respect for u guys bringing this up/ take time to share with us!
But 1 thing strugles me.
This forum teached me that Amfetamine should be white, other colors are (faulty) synthesis related,precursor/ poison leftovers...
I know its common to have a slight color change in the end product, but your end product is just full yellow/orange color ?
Whats the deal about that ?
alteregoHi, alterego!
Yep, that the fact pure Amfetamine have a white color.
The yellow color of Amfetamine is specifically due to its oxidation.
For example, during the evaporation of the solvent at its boiling and during storage with exposure to air.
Additionally, the yellow color can be attributed to impurities of iron salts and sodium sulphate.
In future research, we will study this further and publish new research data.
 
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mithyl2

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Hi, alterego!
Yep, that the fact pure Amfetamine have a white color.
The yellow color of Amfetamine is specifically due to its oxidation.
For example, during the evaporation of the solvent at its boiling and during storage with exposure to air.
Additionally, the yellow color can be attributed to impurities of iron salts and sodium sulphate.
In future research, we will study this further and publish new research data.
GhostChemistI'm very grateful for all of your excellent posts.

would an a/b extraction purify the amphetamine to a white color?
 

UWe9o12jkied91d

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i've done the 'pure white color' amphetamine synth and did indeed obtain a white precipitate at the end.

but do you mean that the white color isn't possible with the P2P synth because of the oxidation?
mithyl2you can recrystalize to fix color(boiling isopropanol and a bit of water) , or a/b, or washing straight after filtering most of the liquid with cold acetone post reaction
be warned with a/b the red contaminants might stay in your organic layer
 

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i've done the 'pure white color' amphetamine synth and did indeed obtain a white precipitate at the end.

but do you mean that the white color isn't possible with the P2P synth because of the oxidation?
mithyl2A white powder is obtained via rinsing anhydrous cold acetone or recrystallization.
But it turns yellow again during prolonged storage.
 

OrgUnikum

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is the purity affected at all by long term storage?
mithyl2It will hold a long time if it is dry, pure, kept cool, away from light and air. Nevertheless there was an article where they examined stored drugs from an old pharmacy which were in a dark cool place for 30 years + and one of the meds was Amphetamine. It had deteriorated to less then half the original amount Amphetamine present over this long time.
Primary Amines are just very reactive even as salts. Amphetamine base deteriorates within hours when subjected to sunlight and 25 °C + in the presence of oxygen (like a bottle with air above the liquid). Best make the salt instantly or keep in a deep-freezer.
 

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Win Win

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Hello! I have 20 liters of p2p, but I can't find a best recipe to experiment with. Is this the best recipe?
 

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Hello! I have 20 liters of p2p, but I can't find a best recipe to experiment with. Is this the best recipe?
Win WinHi!

What do you plan to obtain from p2p? Amphetamine or Methamphetamine?
 
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GhostChemist

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Thanks for your advise…. But you advise this method. I cant do it cuz i cant get N-methylformamide in my place.
Win WinHave you any of the next main reagents for provide conversion p2p to amph or meth: NH3; HgCl2 or other Hg salt; Formamide or ammonium formate; NaBH4 the best variant if you have it; Methylamine Hydrochloride?
 

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Have you any of the next main reagents for provide conversion p2p to amph or meth: NH3; HgCl2 or other Hg salt; Formamide or ammonium formate; NaBH4 the best variant if you have it; Methylamine Hydrochloride?
GhostChemistNH3,HgCI2,NaBH4 and methylamine hydrochloride all this i can get.
 

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mithyl2

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door

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Win Win

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Yes i can
 

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Win WinIn the next step I recomended carried out a trial synthesis of meth for your experimental expirience.
How many g of P2P you willing to trial synthesis?
P2P should be pure (steam distillation will be applied).
You will need of drying agents such as SiO2 (silica gel) and angydrous Na2SO4 (sodium sulphate). Do You have this compounds?
Main reaction carry out in three-necked flask with stirrer and thermometr in ice batch.
 

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Win WinFirst stage: Drying reagents, Imine preparation and Reduction.
Proportions for 10 g of pure P2P (after distillation add SiO2):
1,1 g NaBH4 powder
20 ml of 40% methylamine in methanol (methanol saturated of methylamine) or 23-25 ml of 30% methylamine in IPA
20-50 g or more SiO2
20-30 g or more Na2SO4 angydrous
65-80 ml absolute MeOH or IPA (isopropyl alcohol)
ice bath
ice reserves for a few days
thermometere with range -20 to +50C preferably
Preparing these reagents and flasks for start test working. Need a separate flask with germetic cork for drying of mixture p2p with absolute MeOH or IPA.
Are You understand it?
 

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First stage: Drying reagents, Imine preparation and Reduction.
Proportions for 10 g of pure P2P (after distillation add SiO2):
1,1 g NaBH4 powder
20 ml of 40% methylamine in methanol (methanol saturated of methylamine) or 23-25 ml of 30% methylamine in IPA
20-50 g or more SiO2
20-30 g or more Na2SO4 angydrous
65-80 ml absolute MeOH or IPA (isopropyl alcohol)
ice bath
ice reserves for a few days
thermometere with range -20 to +50C preferably
Preparing these reagents and flasks for start test working. Need a separate flask with germetic cork for drying of mixture p2p with absolute MeOH or IPA.
Are You understand it?
GhostChemistYes i understood
 
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