Reduction MDA Formil Derivative with NaBH4
The synthesis of the starting MDA formyl derivative was presented earlier:
http://bbzzzsvqcrqtki6umym6itiixfhn...phetamine-precursor-for-mdma-synthesis.15218/
http://bbzzzsvqcrqtki6umym6itiixfhn...on/media/mda-formyl-derivative-synthesis.135/
N2 synthesis:
The way of this process approximately proceeds according to Scheme 1 and is accompanied by the formation of an intermediate compound structurally similar to ephedrine.
Scheme 1
Starting reagents and materials
- For N2: 130 g NaNO2 + 230-250 ml H2O + 100 g NH4Cl
- 7.7 g MDA Formil Derivative
- 7.38 g NaBH4
- 100 ml THF
- 550 ml H2O
- 30-50 g NaOH
- 350-400 ml DCM
- 50 ml EtOH
- HCl gas
- 50-70 ml Petroleum ether
- pH-indicator strips
- Filter papers
- Beakers
- Flasks
- Dropping funnel
- Heaters
7.38 g of NaBH4 and 50 ml dry THF were placed in the flask Fig 1
Fig 1
The system is purged with dry nitrogen. Fig 2
Fig 2
Formation of nitrogen during the reaction of ammonium chloride with sodium nitrite (the reaction is exothermic!) Fig 3
Fig 3
Mixture of NaBH4 and THF heated to 50-60℃ Fig 4
Fig 4
Solution of 7.7 g MDA Formil Derivative in 50 ml THF was prepared. Fig 5
Fig 5
Solution of MDA Formil Derivative in THF was placed into dropping funnel Fig 6
Fig 6
Solution of MDA Formil Derivative in THF was added by drops to NaBH4. H2 was formed after added MDA Formil Derivative! Fig 7
Fig 7
RM is stirring at 50-60℃ for 4 days. Fig 8
Fig 8
RM was cooled to room temperature and transferred into beaker Fig 9
Fig 9
250 ml of water is added to RM. рН is alkali Fig 10
Fig 10
300 ml of (30-50 г NaOH) NaOH solution is added too Fig 11
Fig 11
The solution was placed into a separatory funnel, and DCM extraction was done. Fig 12
Fig 12
The summary volume of DCM is 400 ml Fig 13
Fig 13
DCM is dried with sodium sulphate Fig 14
Fig 14
DCM is distilled off. Oil in the flask Fig 15
Fig 15
The oil is dissolved in EtOH (50 ml) and filtered through the paper filter Fig 16
Fig 16
Solution has alkali pH Fig 17
Fig 17
Needle-shaped crystals are formed in the solution Fig 18
Fig 18
HCl is bubbled through the solution to acidic pH Fig 19
Fig 19
The solution evaporates to half its volume Fig 20
Fig 20
After cooled to room temperature, the crystals were formed. Crystallization ends after a few hours Fig 21
Fig 21
To the white precipitate is added petroleum ether Fig 22
Fig 22
Precipitate is filtered and dried Fig 23
Fig 23
Yield is 6 g Fig 24
Fig 24
Further reduction of the obtained compound, which contained a methylenedioxy group, with iodine and hypophosphoric acid, similar to the process of reduction of ephedrine (http://bbzzzsvqcrqtki6umym6itiixfhn...s-from-ephedrine-by-using-i2-and-h3po2.10423/), leads to the destruction of the methylenedioxy group without the formation of the MDMA and the formation of by-products as resins. Scheme 2
Scheme 2
During the reaction, RM turns black and resinifies, and chemical analysis with gallic acid shows the destruction of the methylenedioxy group. (
) Fig 25
Fig 25