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Synthesis of Dextroamphetamine from P2P with (S)-(−)-α-Methylbenzylamine (1000g scale)

William Dampier

Well-known member
Jul 19, 2021
Reaction score
Step 1. Reductive amination of P2P.

1. Phenylacetone (1000 g) and (S)-(−)-α-Methylbenzylamine (904 g) added in flask.
2. Stirred at room temperature, 10-15 min.
3. To the reaction mixture was added slowly sodium borhydride (282 g).
4. After was added boric acid (461 g) (can replace p-toluenesulfonic acid monohydrate (1418 g) or benzoic acid (911 g)).
5. The reaction mixture was stirred 1 hour at room temperature.
6. After was quenched with saturated aqueous solution of NaHCO3 to alkaline pH.
7. Extracted with CH2Cl2 or ether.
8. Extract was dried over anhydrous Na2SO4, filtered and concentrated to get N-benzylamphetamine base.

Step 2. Debenzylation.

1. Formic acid (1026 g), KOH (1251 g), N-benzylamphetamine base (1000 g) and ethanol (5 liters) added in flask.
2. The reaction mixture was heated at reflux conditions.
3. 475g Pd/C 10% catalyst was added to the heated reaction mixture.

4. It was stirred at reflux for 60 min.
5. After the reaction, the mixture was cooled to room temperature and filtered.
6. Ethanol solution was evaporated to get amphetamine base.
7. The catalyst on filter was collected, washed twice with water and once again with ethanol.
8. The isolated catalyst was used in the next cycle.

Step 3. Precipitation.
1. Base from Step 2.6 dissolved in 2 liters acetone and stirring.
2. Sulfuric acid was added dropwise to solution to pH - 6.

3. Put in the freezer for 12 hours.
4. After this time, mixture filtered and dried on air to get amphetamine sulfate.
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