1,1'-Carbonyldiimidazole → 3-(2,4-Difluorophenyl)-1,5-dimethyl-6-thioxo-[1,3,5]triazinane-2,4-dione

Participants

Reaction Conditions

Reaction Steps

31 g of 2,4-difluorophenyl isocyanate and 64.9 g of carbodiimidazole were added in succession to 20.8 g of N,N′-dimethylthiourea in 500 ml of toluene and 1 ml of triethylamine. This mixture was stirred first for 3 hours at 60-65° C. and then for 12 hours at 80-85° C. After cooling to room temperature, the mixture was washed three times with 100-ml-portions of water, and the organic phase was dried over sodium sulfate. After distillation of the low-boiling fractions, 48 g of the desired product of melting point 156-159° C. remained.

Provenance & Evidence