Experimental section. The synthesis of the Amphetamine sulphate using P2P with ammonium acetate and reduction with Mg

GhostChemist

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The reactions proceed according to Scheme 1.
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Scheme 1.

Starting reagents and materials
  • 5 g purified P2P (P2P obtained through the reduction of P2NP with sodium borohydride and steam distill)
  • 4.1 g Mg
  • 37 г H3CCOONH4 (CAS 631-61-8)
  • 250-300 ml H2O
  • 80 ml EtOH 88%
  • 30 ml HAc
  • 500 ml DCM
  • 5+5 ml Ethyl acetate
  • 1-2 mL of concentrated sulfuric acid (83%)
  • pH indicator paper
  • 50 g of anhydrous sodium sulfate
  • 50 mL of 25% NaOH (sodium hydroxide)
  • Flasks
  • Reflux condenser
  • Separatory funnel
  • Filter paper
  • Funnels
  • Beakers
  • Heater
In Figure 1, the starting components are presented.
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Fig 1
P2P is placed into a 1 L flask along with ammonium acetate and ethanol, and the mixture is well stirred. Fig 2
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Fig 2
Small portins of Mg is added to the obtained mixture. Fig 3
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Fig 3
During the reaction, portions 5-10 ml of acetic acid (HAc) is added. Fig 4
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Fig 4
The reaction proceeds smoothly and does not require cooling. The reaction is completed within 3-4 hours. Fig 5
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Fig 5

The RM after reaction finished. Fig 6
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Fig 6

After the reaction is complete, the mixture is filtered. Fig 7
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Fig 7

Next, a 50 ml of 25% aqueous solution of NaOH is added until the pH reaches 8-10. During this process, a white precipitate of magnesium hydroxide will form, accompanied by the release of the amphetamine as a free base, characterized by a distinctive pleasant odor. Fig 8
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Fig 8

100 mL of DCM is added to the filtrate for the extraction of the aphetamine free base. Fig 9
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Fig 9

The amphetamine free base from RM is further extracted with several portions of DCM. If the reaction mass is too dense, water is added to dilute it. Fig 10
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Fig 10

The extract in DCM is dried with anhydrous sodium sulfate. Fig 11
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Fig 11

The drained extract of amphetamine in DCM. Fig 12
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Fig 12

After DCM distilled off, the flask contains the oil of the amphetamine free base. Fig 13
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Fig 13

Ethyl acetate added to the aphetamine free base and filtered to a glass beaker, and the residues in the flask are washed with 5 mL of ethyl acetate. Fig 14
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Fig 14

Sulfuric acid is added to the aphetamine free base solution in ethyl acetate until the pH 7. A precipitate of aphetamine sulfate is forming. Fig 15
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Fig 15

The precipitate of aphetamine sulfate is filtered through a paper filter and washed with 5 mL of ethyl acetate. The precipitate was air-dried. Fig 16
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Fig 16



The yield of amine sulfate was 0.86 g or 12.5%
 
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