반응 #2065334

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
   기타at 25° C
2. 2
   여과The precipitate was filtered off with suction
3. 3
   추출the organic phase was extracted 3× with water
4. 4
   기타dried
5. 5
   기타evaporated

실험 절차

4.7 g (0.278 mol) of gaseous ammonia were passed over the course of 1 hour into a stirred mixture of 38.0 g (0.147 mol) of 2-fluoro(chloro)-4-trifluoromethoxy-6-trifluoromethylpyrimidine and 150 ml of diethyl ether at −75 to −70° C. The mixture was stirred for 2 hours each at −75 and at 25° C. The precipitate was filtered off with suction, and the organic phase was extracted 3× with water, dried and evaporated. Chromatography on silica gel with methyl tert.-butyl ether yielded 20.4 g (56.1% of theory) of the title compound of melting point 47-49° C.

출처