반응 #1857546

반응 방정식

hydrochloric acid

1,2,4-Triazole

2-bromo-1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone

sodium hydride

→

desired material

수율 80.3%

1-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-(1,2,4-triazol-1-yl)ethanone

수율 80.3%

용매

water

THF

THF

반응 조건

후처리

1. 1
   workup.ADDITIONwas added (3000 mL)
2. 2
   여과The precipitate was filtered off
3. 3
   세척washed with MTBE
4. 4
   농축The organic phase was then concentrated
5. 5
   여과the resulting solid was filtered off

실험 절차

1,2,4-Triazole (249 g) was added carefully (small portions) to a mixture of sodium hydride (85 g) in THF (6000 mL). After 30 minutes a solution of 2-bromo-1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone (1322 g) in THF (500 mL) was slowly added and the mixture was stirred for 150 min. The pH was adjusted to 7 with dil. hydrochloric acid whereupon water was added (3000 mL). The precipitate was filtered off and washed with MTBE. The organic phase was then concentrated and the resulting solid was filtered off to yield the desired material (1008 g).

출처