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Old methods for synthesizing DOB

Joni

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We make DOB from amine.

How to make a short tutorial out of this?

Evaporate the IPA, get a thick oily mucus or oil (if you're lucky) yellow. It is the pure amine base. It is dissolved in a strictly measured small amount of glacial acetic acid, the solution is weighed. From the resulting mass subtract the mass of glacial acetic acid, the mass of the amine remains. I don't know how to weigh the recovery result differently.

Glacial acetic acid is added so that 10 ml of acid per 5 g of amine. Dissolve bromine, equal in mass to the amine, in 10 ml of glacial acetic acid. Add the bromine solution to the amine solution. The reaction is slightly exothermic. DOB (when 2,5-substituted nitropropene was reduced), the resulting solution was stirred at room temperature for 3 hours, after which it was diluted with 150...250 ml of water, while the turbidity increased significantly. The mixture is washed with 100 ml of ether, alkalized to pH>12 with an aqueous solution of NaOH, extracted with three portions of 100 ml of dichloromethane. The combined extracts are washed with water and the dichloromethane is evaporated off.

The resulting thick yellow oil is dissolved in 150...250 ml of ether and HCl gas is passed through. White flakes begin to fall out. The process is controlled by acidity, and when pH=7 is reached, the gas supply is stopped. The crystals are filtered off, and the passage of gas is resumed through the liquid. When flocculation has ceased, the gas is removed, the crystals are filtered off, combined with those previously collected and dried.
Recrystallize (optional) from IPA. The output is usually 75...85%. The result was one of the most potent psychedelics - DOB, in the form of hydrochloride. In no case should you taste it without looking at the dosages: literally a few grains tear the roof apart, and this goes on longer than a person can bear!
 
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