反应详情

温度

-70 °C

At -75° to -70° C. and over a period of 1 hour, 8.7 g (0.51 mol) of gaseous ammonia was gassed, while stirring, into a mixture of 51 g (0.255 mol) of 2,4-difluoro-6-trifluoromethoxypyrimidine in 200 ml of diethyl ether. The mixture was stirred for 1 1/2 hours at -70° C. and for 1 hour at room temperature. The reaction mixture was evaporated down under reduced pressure, taken up in methylene chloride and extracted with water. The organic phase was dried, evaporated down and chromatographed over silica gel (8:1 ligroin/ether mixture) to give 38.1 g (75.6% of theory) of the title compound as colorless crystals of melting point 86°-89° C.

1. customThe reaction mixture was evaporated down under reduced pressure
2. extractionextracted with water
3. customThe organic phase was dried
4. customevaporated down
5. customchromatographed over silica gel (8:1 ligroin/ether mixture)