反応 #50644

反応方程式

trichloroacetyl chloride

(E)-3-chloro-2-fluoro-cinnamamide oxime

pyridine

→

(E)-3-(3-chloro-2-fluoro-styryl)-5-trichloromethyl-1,2,4-oxadiazole

収率 48.7%

溶媒

chloroform

反応条件

後処理

1. 1
   温度of heat
2. 2
   ろ過the pyridine hydrochloride which separates out is filtered off
3. 3
   洗浄washed with chloroform
4. 4
   濃縮The filtrate is concentrated in vacuo
5. 5
   その他the remaining solid material is recrystallized

実験手順

12.7 g (0.07 mol) of trichloroacetyl chloride are added dropwise to a suspension consisting of 6.4 g (0.03 mol) of (E)-3-chloro-2-fluoro-cinnamamide oxime in 90 ml of chloroform and 6 ml (0.07 mol) of dry pyridine. During this process, there is a slight evolution of heat. Subsequently, the mixture is stirred for 1 hour and the pyridine hydrochloride which separates out is filtered off and washed with chloroform. The filtrate is concentrated in vacuo and the remaining solid material is recrystallized. 5.0 g (48.7% of theory) of (E)-3-(3-chloro-2-fluoro-styryl)-5-trichloromethyl-1,2,4-oxadiazole are obtained.

出典