反应详情

温度

62.5 °C

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.

1. waitfor 12 hours at 80-85° C
2. temperatureAfter cooling to room temperature
3. washthe mixture was washed three times with 100-ml-portions of water
4. dry with materialthe organic phase was dried over sodium sulfate
5. distillationAfter distillation of the low-boiling fractions, 48 g of the desired product of melting point 156-159° C.