HRID1646463

反应详情

EQUATION

反应方程式

HRID 1646463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 12.5 g of 2-(5-amino-2-chloro-4-fluorophenylthio)-4-chlorobutyric acid ethyl ester, 10.6 g of potassium carbonate and 0.7 g of tetrabutylammonium hydrogen sulfate in 14 ml of toluene is maintained at +80° C. for 40 hours. The solid portions of the reaction mixture are then filtered off and washed with acetone. Evaporation of the solvent and recrystallisation from n-hexane and a small amount of ethyl acetate yield 7.9 g of 1-(5-amino-2-chloro-4-fluoro-phenylthio)-cyclopropanecarboxylic acid ethyl ester having a melting point of from +96° to +97° C.

WORKUP

后处理

  1. temperatureis maintained at +80° C. for 40 hours
  2. filtrationThe solid portions of the reaction mixture are then filtered off
  3. washwashed with acetone
  4. customEvaporation of the solvent and recrystallisation from n-hexane
  5. customof from +96° to +97° C.