HRID2072685

反应详情

EQUATION

反应方程式

HRID 2072685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.58 g of 4-[3-chloro-4-(ethoxycarbonylmethoxy)phenyl]-4-oxobutyric acid [prepared as described in step (a) above] was dissolved in 10 ml of ethanol and 0.31 g of 80% v/v aqueous hydrazine hydrate was added thereto, whilst ice-cooling. The mixture was stirred, with ice-cooling, for 5 minutes, and then heated under reflux for 3 hours, after which ethyl acetate was added thereto. The mixture was then cooled to room temperature and the resulting precipitate was recrystallized from a mixture of ethyl acetate and hexane, to give 1.49 g of the title compound, having the same characteristics as the product of Example 1.

WORKUP

后处理

  1. temperaturewhilst ice-cooling
  2. temperaturecooling, for 5 minutes
  3. temperatureheated
  4. temperatureunder reflux for 3 hours
  5. customthe resulting precipitate was recrystallized from a mixture of ethyl acetate and hexane