반응 #50646

반응 방정식

potassium hydroxide

diethyl cyanomethylphosphonate

4-chloro-3-trifluoromethylbenzaldehyde

→

4-chloro-3-trifluoromethyl-cinnamonitrile

수율 87.1%

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   온도of heat
2. 2
   여과is filtered off
3. 3
   세척washed with tetrahydrofuran
4. 4
   농축The filtrate is concentrated in vacuo
5. 5
   기타the remaining residue is dried

실험 절차

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.

출처