GhostChemist
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The process of the free base formation process proceeds according to Scheme 1
Reagents and materials
A solution of alkali in water is prepared in advance and cooled to room temperature. Fig 1
300 ml of water is added to the MDA hydrochloride and mixed well. Fig 2
The cooled alkali solution is added to the MDA hydrochloride solution. Fig 3
The resulting mixture is transferred to a separatory funnel. Fig 4
When a distinct lower layer appears, the DCM is drained and the extraction is repeated. Fig 6
DCM is distilled off to the oil. Fig 8
Oil weight 40 g (yield 97%) Fig 9
Place 20 g of Oil in a glass Fig 10
Petroleum ether 25 ml and 2-5 g of aluminum oxide are added to the oil. The mixture is stirred well. Fig 11
Filter the aluminum oxide and wash with additional portions of petroleum ether. Fig 12
The formation of MDA hydrochloride from the free base proceeds according to Scheme 2
The pH should become slightly acidic, with the orange oil turning into a flesh-colored sediment. Fig 14
Scheme 1โ
Reagents and materials
- 49.6 g MDA*HCl + 300 ml H2O
- 30 g NaOH + 300 ml H2O
- 800-1000 ml DCM
- 2-5 g Al2O3
- 150-200 ml Petroleum ether
- Flasks
- Beakers
- Reflux
- Separating funnel 2000 ml
- Heating mantle
- pH-indicator paper
- Filter paper
- HCl gas
- Distillation setup
- Vacuum filter
Extraction of Free Baseโ
A solution of alkali in water is prepared in advance and cooled to room temperature. Fig 1
Fig 1โ
300 ml of water is added to the MDA hydrochloride and mixed well. Fig 2
Fig 2โ
The cooled alkali solution is added to the MDA hydrochloride solution. Fig 3
Fig 3โ
The resulting mixture is transferred to a separatory funnel. Fig 4
Fig 4โ
DCM is added to the solution in portions until the layers are clearly separated. If the layers are not separated well, can be adding 400 ml of water and then DCM again. The mixture is mixed well. Fig 5โ
Fig 5โ
When a distinct lower layer appears, the DCM is drained and the extraction is repeated. Fig 6
Fig 6โ
The DCM layer is dried with anhydrous sodium sulfate. If there are suspended particles not absorbed by sodium sulfate, the solution is additionally filtered before distillation. Fig 7โ
Fig 7โ
DCM is distilled off to the oil. Fig 8
Fig 8โ
Oil weight 40 g (yield 97%) Fig 9
Fig 9โ
Place 20 g of Oil in a glass Fig 10
Fig 10โ
Petroleum ether 25 ml and 2-5 g of aluminum oxide are added to the oil. The mixture is stirred well. Fig 11
Fig 11โ
Filter the aluminum oxide and wash with additional portions of petroleum ether. Fig 12
Fig 12โ
MDA Hydrochloride Formationโ
The formation of MDA hydrochloride from the free base proceeds according to Scheme 2
Scheme 2โ
An additional 20 ml of petroleum ether is added to the filtered solution. Saturation with hydrogen chloride is carried out, with petroleum ether periodically added to replace the evaporating one. Fig 13โ
Fig 13โ
The pH should become slightly acidic, with the orange oil turning into a flesh-colored sediment. Fig 14
Fig 14โ
Filter the resulting precipitate, if necessary, rinse additionally with DCM. Fig 15โ
Fig 15โ
Yield of MDA*HCl is 20.4 g or 84.8%
Fig 16โ
Fig 16โ
Fig 16โ