تفاعل #50646

معادلة التفاعل

potassium hydroxide

diethyl cyanomethylphosphonate

4-chloro-3-trifluoromethylbenzaldehyde

→

4-chloro-3-trifluoromethyl-cinnamonitrile

المردود 87.1%

المذيبات

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةof heat
2. 2
   ترشيحis filtered off
3. 3
   غسيلwashed with tetrahydrofuran
4. 4
   تركيزThe filtrate is concentrated in vacuo
5. 5
   أخرىthe remaining residue is dried

الإجراء التجريبي

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.

المصدر