반응 #1284596

반응 방정식

ammonia

2-fluoro(chloro)-4-trifluoromethoxy-6-trifluoromethylpyrimidine

→

title compound

2-Amino-4-trifluoromethoxy-6-trifluoromethylpyrimidine

용매

diethyl ether

반응 조건

후처리

1. 1
   여과filtered
2. 2
   추출the organic phase was extracted with water
3. 3
   기타dried
4. 4
   기타partially evaporated down

실험 절차

At -75° to -70° C. and over a period of 1 hour, 4.7 g (0.278 mol) of gaseous ammonia was gassed, while stirring, into a mixture of 38.0 g (0.147 mol) of 2-fluoro(chloro)-4-trifluoromethoxy-6-trifluoromethylpyrimidine in 150 ml of diethyl ether. The mixture was stirred for 2 hours at -75° C. and for 2 hours at 25° C. The precipitate was suction filtered, and the organic phase was extracted with water, dried and partially evaporated down. Chromatography with methyl tert-butyl ether over silica gel gave 20.4 g (56.1% of theory) of the title compound of melting point 47°-49° C.

출처