反応 #50646

反応方程式

potassium hydroxide

diethyl cyanomethylphosphonate

4-chloro-3-trifluoromethylbenzaldehyde

→

4-chloro-3-trifluoromethyl-cinnamonitrile

収率 87.1%

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度of heat
2. 2
   ろ過is filtered off
3. 3
   洗浄washed with tetrahydrofuran
4. 4
   濃縮The filtrate is concentrated in vacuo
5. 5
   その他the remaining residue is dried

実験手順

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.

出典