Hydrochloric Acid → 2,4-Dichloro-6-methyl-1,3,5-triazine

Participants

Reaction Conditions

Reaction Steps

In a 2 l flask equipped with a mechanical stirrer, a dry ice condenser, a thermometer and a gas inlet was charged 700 ml of toluene and 50 g of N-methylacetamide. It was cooled to 10° C. and then was charged 60 g of phosgene at 10°-20° C. Afterwards, 30 g of HCl gas was introduced. Then, 50 g of sodium dicyanamide was charged in one portion and the HCl charge continued until 56 g of total HCl was introduced. The reaction mass was heated to 65° C. for 2 hours. After cooling to 20° C., the reaction content consisted of toluene and some tars. The toluene phase was decanted into 500 ml of ice water. The residue was rinsed with 300 ml of toluene and then decanted. The combined toluenes were washed with water (2×500 ml) and dried over MgSO4. After evaporation, 32.5 g of 2,4-dichloro-6-methyl-1,3,5-triazine was obtained as white needles (35% yield).

Provenance & Evidence