HRID1646467

反应详情

EQUATION

反应方程式

HRID 1646467 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

While stirring at room temperature, a solution of 5.5 g of 1-(5-amino-2-chloro-4-fluoro-phenylthio)-cyclopropanecarboxylic acid methyl ester in 20 ml of ethylene chloride is added dropwise to a mixture of 3 g of calcium carbonate, 2 ml of thiophosgene in 20 ml of ethylene chloride and 20 ml of water. After stirring for 4 hours at room temperature, the inorganic portion of the reaction mixture is filtered off and the organic phase is dried over calcium chloride and then concentrated by evaporation, yielding 6.3 g of 1-(2-chloro-4-fluoro-5-isothiocyanato-phenylthio)-cyclopropanecarboxylic acid methyl ester having a melting point of from +100° to +101° C.

WORKUP

后处理

  1. stirringAfter stirring for 4 hours at room temperature
  2. filtrationthe inorganic portion of the reaction mixture is filtered off
  3. dry with materialthe organic phase is dried over calcium chloride
  4. concentrationconcentrated by evaporation