Reactions proceed according to Scheme 1
In two separate beakers, hydroxylamine hydrochloride and sodium hydroxide are mixed with ethanol or IPA. Fig 2
Next, the contents of the beakers are combined. Fig 3
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
Next, aluminum amalgam is prepared using the standard method. Fig 5
The reaction is fully completed within 1-1.5 hours. Fig 8
The reaction mass is filtered through a paper filter. Fig 9
The filtered DСM is dried with anhydrous sodium sulfate. Fig 11
DCM is distilled off at a temperature of 90°C. Fig 12
After distillation, a yellow-colored oil remains in the residue. Fig 13
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
Sulfuric acid is added to the obtained amphetamine solution until the pH reaches 5-6, resulting in the precipitation of amphetamine sulfate. Fig 15
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
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 1In two separate beakers, hydroxylamine hydrochloride and sodium hydroxide are mixed with ethanol or IPA. Fig 2
Next, the contents of the beakers are combined. Fig 3
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
Next, aluminum amalgam is prepared using the standard method. Fig 5
The prepared P2P oxime solution is added to the resulting aluminum amalgam, and a reflux condenser is connected. Fig 6
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
The reaction is fully completed within 1-1.5 hours. Fig 8
The reaction mass is filtered through a paper filter. Fig 9
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
The filtered DСM is dried with anhydrous sodium sulfate. Fig 11
DCM is distilled off at a temperature of 90°C. Fig 12
After distillation, a yellow-colored oil remains in the residue. Fig 13
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
Sulfuric acid is added to the obtained amphetamine solution until the pH reaches 5-6, resulting in the precipitation of amphetamine sulfate. Fig 15
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
The yield of amphetamine sulfate is 2.5 g, which corresponds to 36%.
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