HRID637943

反应详情

EQUATION

反应方程式

HRID 637943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.3 g of cyclopropylamine are added dropwise to a solution of 24.9 g of ethyl 2-(2,4-dichloro-5-fluorobenzoyl)-3-ethoxy-acrylate (5) in 80 ml of ethanol, while cooling with ice and stirring. When the exothermic reaction has subsided, the mixture is stirred for a further hour at room temperature, the solvent is stripped off in vacuo and the residue is recrystallised from cyclohexane/petroleum ether. 22.9 g of ethyl 2-(2,4-dichloro-5-fluoro-benzoyl)-3-cyclopropylamino-acrylate (6) of melting point 89° to 90° C. are obtained.

WORKUP

后处理

  1. temperaturewhile cooling with ice
  2. customWhen the exothermic reaction
  3. stirringthe mixture is stirred for a further hour at room temperature
  4. customthe residue is recrystallised from cyclohexane/petroleum ether