反应 #1857546

反应方程式

hydrochloric acid

1,2,4-Triazole

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

sodium hydride

→

desired material

收率 80.3%

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

收率 80.3%

溶剂

water

THF

THF

反应条件

后处理

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

实验过程

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).

来源