반응 #319703

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
   workup.STIRRINGStirring
2. 2
   workup.WAITwas continued for 2 hours in each case at -75° C.
3. 3
   기타The precipitate which separated out
4. 4
   여과was filtered off under suction
5. 5
   추출after which the organic phase was extracted with water
6. 6
   기타dried
7. 7
   기타partially evaporated down

실험 절차

4.7 g (0.278 mol) of gaseous ammonia were passed into a mixture of 38.0 g (0.147 mol) of 2-fluoro(chloro)-4-trifluoromethoxy-6-trifluoromethylpyrimidine in 150 ml of diethyl ether while stirring at from -75° to -70° C. in the course of 1 hour. Stirring was continued for 2 hours in each case at -75° C. and, after heating, at 25° C. The precipitate which separated out was filtered off under suction, after which the organic phase was extracted with water, dried and partially evaporated down. Chromatography over silica gel using methyl tert-butyl ether gave 20.4 g (56.1% of theory) of the title compound of melting point 47°-49° C.

출처