Hydrochloric Acid → 4-Methoxy-6-(trifluoromethyl)-1,3,5-triazin-2-amine

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Reaction Steps

56.6 g (0.5 mol) of calcium chloride (98%, powdered) and 210 g (2.5 mol) of N-cyanoguanidine are initially introduced into 2 l of methanol. The mixture is heated with stirring to reflux temperature and stirred under reflux for one hour, whereupon a homogeneous solution is obtained. The mixture is then cooled to room temperature and 640 g (5.0 mol) of methyl trifluoroacetate and then, in the course of 25 minutes, 450 g (2.5 mol) of a solution of sodium methoxide (30% by weight in methanol) are added, whereupon a white precipitate deposits. After heating under reflux for 2 hours, the mixture is cooled to room temperature and a pH of about 6 is set by addition of conc. hydrochloric acid. The methanol is then distilled off, about 2 l of water are added little by little, and the deposited, finely crystalline white crystals are separated off and dried in vacuo.

Provenance & Evidence