Express Return Method for Obtain Amphetamine sulphate

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Express return method for obtain Amp sulphate

General scheme of the processes. Scheme 1

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Scheme 1

Starting reagents and materials

  • 3 g AMP sulfate
  • 50-100 ml IPA
  • 20 ml IPA + H2SO4 (concentration unknown)
  • 30-60 g NaOH
  • 200-250 ml H2O
  • Beakers
  • Separating funnel 250 ml
  • Pipettes
  • pH-indicator strips
  • Filters
The process of A sulfate solubility in solution of H2SO4 in IPA. Scheme 2
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Scheme 2

A sulphate is placed into a beaker Fig 1

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Fig 1

A solution of ~25% sodium hydroxide is prepared (30 g in 100-120 ml H2O) Fig 2

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Fig 2

20-25 ml of IPA is added to the A sulfate. Fig 3

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Fig 3

Sulfuric acid solution in IPA is added dropwise until A sulfate is dissolved (Scheme 2) Fig 4

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Fig 4

The formation of the free base occurs according to Scheme 3

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Scheme 3

An alkali solution is added to the A hydrosulfate solution. Fig 5

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Fig 5

25-50 ml of IPA is added to the resulting mixture. Fig 6

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Fig 6

The mixture is transferred to a separatory funnel and the upper layer of IPA containing free base A is separated. If separation is poor, an additional portion of alkali (25-30% solution) and IPA is added. Fig 7

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Fig 7

The formation of sulfate A again is shown in Scheme 4.

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Scheme 4

A solution of sulfuric acid in IPA is slowly added to the IPA layer with constant stirring, drop by drop, until the mixture reaches a neutral reaction. Fig 8

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Fig 8

The mixture should have a neutral pH. Fig 9

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Fig 9
The resulting precipitate was filtered off. Fig 10
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Fig 10

The precipitate is dried on the filter Fig 11

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Fig 11

Yield 2.95-3 g Fig 12

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Fig 12


Confirmation of consist A - adding a granule of alkali to the sample and a drop of water - a specific smell of the free base should appear

The impurity will be an inert and safe salt - sodium sulfate.

To obtain a purer product, distillation of the free base with steam is used.


 
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