HRID1646459

反应详情

EQUATION

反应方程式

HRID 1646459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.4 g of 1-(5-amino-2-chloro-4-fluoro-phenylthio)-cyclopropanecarboxylic acid, 1.5 g of 3,4,5,6-tetrahydrophthalic anhydride and 100 ml of glacial acetic acid is heated under reflux for 18 hours while stirring. The reaction mixture is then introduced into ice-water and the resulting product is extracted with ethyl acetate. Drying over sodium sulfate and concentration of the solution by evaporation yield 1.7 g of 1-[2-chloro-4-fluoro-5-(1,2,3,4,5,6-hexahydro-1,3-dioxo-isoindolyl)-phenylthio]-cyclopropanecarboxylic acid having a melting point of from +186° to +188° C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 18 hours
  3. extractionthe resulting product is extracted with ethyl acetate
  4. dry with materialDrying over sodium sulfate and concentration of the solution by evaporation yield 1.7 g of 1-[2-chloro-4-fluoro-5-(1,2,3,4,5,6-hexahydro-1,3-dioxo-isoindolyl)-phenylthio]-cyclopropanecarboxylic acid having a melting point of from +186° to +188° C.