反应 #50646

反应方程式

potassium hydroxide

diethyl cyanomethylphosphonate

4-chloro-3-trifluoromethylbenzaldehyde

→

4-chloro-3-trifluoromethyl-cinnamonitrile

收率 87.1%

溶剂

tetrahydrofuran

tetrahydrofuran

反应条件

后处理

1. 1
   温度of heat
2. 2
   过滤is filtered off
3. 3
   洗涤washed with tetrahydrofuran
4. 4
   浓缩The filtrate is concentrated in vacuo
5. 5
   其他the remaining residue is dried

实验过程

A solution consisting of 10.6 g (0.06 mol) of diethyl cyanomethylphosphonate and 12.5 g (0.06 mol) of 4-chloro-3-trifluoromethylbenzaldehyde in 65 ml of tetrahydrofuran is added dropwise to a suspension of 6.7 g (0.12 mol) of powdered potassium hydroxide in 185 ml of tetrahydrofuran. During this process, there is a slight evolution of heat. Subsequently, the mixture is stirred at room temperature for 20 minutes and the solid material which separates off is filtered off and washed with tetrahydrofuran. The filtrate is concentrated in vacuo and the remaining residue is dried. 12.1 g (87.0% of theory) of 4-chloro-3-trifluoromethyl-cinnamonitrile are obtained as an E/Z isomeric mixture.

来源