HRID2072023

反应详情

EQUATION

反应方程式

HRID 2072023 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

2-Chloro-3-((4-(2,2-dichloro-1,1-difluoroethoxy)phenyl)sulfonyl)propanenitrile (hereinafter "Compound") is prepared by mixing together 4-(2,2-dichloro-1,1-difluoroethoxy)benzenesulfonyl chloride with substantially two molecular proportions of acrylonitrile in the presence of acetonitrile, cupric chloride and triethylamine hydrochloride whereby the following reaction takes place: ##STR1## In the process, 4-(2,2-dichloro-1,1-difluoroethoxy)-benzenesulfonyl chloride (1 molar proportion), acrylonitrile (2 molar proportions), acetonitrile, anhydrous cupric chloride (.02 molar proportion) and triethylamine hydrochloride (0.032 molar proportion) are placed in a reaction vessel which is cooled, evacuated to about 2 mm mercury pressure, sealed and heated in an oil bath at about 115° C. for about six hours. The vessel is opened and the product is isolated by crystallization from methanol to give the title compound as a white, crystalline solid, melting at 109° C.

WORKUP

后处理

  1. customthe following reaction
  2. temperaturewhich is cooled
  3. customevacuated to about 2 mm mercury pressure
  4. customsealed
  5. customthe product is isolated by crystallization from methanol