Реакция #50644

ord-ee72f4837e0f489eb3d751852d9ce809

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураof heat
  2. 2
    Фильтрацияthe pyridine hydrochloride which separates out is filtered off
  3. 3
    Промывкаwashed with chloroform
  4. 4
    КонцентрированиеThe filtrate is concentrated in vacuo
  5. 5
    Другоеthe remaining solid material is recrystallized

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05428049uspto-grants-1995_06