3,4-Methylenedioxyamphetamine (MDA) Purification Method

[GhostChemist]

The process of the free base formation process proceeds according to Scheme 1

Scheme 1​

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 Base​

A solution of alkali in water is prepared in advance and cooled to room temperature. Fig 1

Fig 1​

300 ml of water is added to the MDA hydrochloride and mixed well. Fig 2

Fig 2​

The cooled alkali solution is added to the MDA hydrochloride solution. Fig 3

Fig 3​

The resulting mixture is transferred to a separatory funnel. Fig 4

Fig 4​

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 5​

Fig 5​

When a distinct lower layer appears, the DCM is drained and the extraction is repeated. Fig 6

Fig 6​

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 7​

Fig 7​

DCM is distilled off to the oil. Fig 8

Fig 8​

Oil weight 40 g (yield 97%) Fig 9

Fig 9​

Place 20 g of Oil in a glass Fig 10

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

Fig 11​

Filter the aluminum oxide and wash with additional portions of petroleum ether. Fig 12

Fig 12​

MDA Hydrochloride Formation​

The formation of MDA hydrochloride from the free base proceeds according to Scheme 2

Scheme 2​

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 13​

Fig 13​

The pH should become slightly acidic, with the orange oil turning into a flesh-colored sediment. Fig 14

Fig 14​

Filter the resulting precipitate, if necessary, rinse additionally with DCM. Fig 15​

Fig 15​

Yield of MDA*HCl is 20.4 g or 84.8%
Fig 16​

Fig 16​

 

[Mo0odi]

I hope you make a video of all your work so it can be a reference for us.

Thank you

 

[HIGGS BOSSON]

The video is being edited

 

[Mo0odi]

Thanks