Reduction MDA Formil Derivative with NaBH4

[GhostChemist]

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​