GhostChemist
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Express return method for obtain Amp sulphate
General scheme of the processes. Scheme 1
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
Scheme 2
A sulphate is placed into a beaker Fig 1
Fig 1
A solution of ~25% sodium hydroxide is prepared (30 g in 100-120 ml H2O) Fig 2
Fig 2
20-25 ml of IPA is added to the A sulfate. Fig 3
Fig 3
Sulfuric acid solution in IPA is added dropwise until A sulfate is dissolved (Scheme 2) Fig 4
Fig 4
The formation of the free base occurs according to Scheme 3
Scheme 3
An alkali solution is added to the A hydrosulfate solution. Fig 5
Fig 5
25-50 ml of IPA is added to the resulting mixture. Fig 6
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
Fig 7
The formation of sulfate A again is shown in Scheme 4.
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
Fig 8
The mixture should have a neutral pH. Fig 9
Fig 9
Fig 10
The precipitate is dried on the filter Fig 11
Fig 11
Yield 2.95-3 g Fig 12
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.