反応 #1857546

反応方程式

hydrochloric acid

1,2,4-Triazole

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

sodium hydride

→

desired material

収率 80.3%

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

収率 80.3%

溶媒

water

THF

THF

反応条件

後処理

1. 1
   workup.ADDITIONwas added (3000 mL)
2. 2
   ろ過The precipitate was filtered off
3. 3
   洗浄washed with MTBE
4. 4
   濃縮The organic phase was then concentrated
5. 5
   ろ過the resulting solid was filtered off

実験手順

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).

出典