반응 #1734862

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
   기타The precipitate which had separated out
3. 3
   여과was filtered off under suction
4. 4
   추출after which the organic phase was extracted with water
5. 5
   기타dried
6. 6
   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 in the course of 1 hour at from -75° to -70° C. while stirring. Stirring was continued for 2 hours at -75° C. and for 2 hours after warming up to 25° C. The precipitate which had 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