HRID220684

反应详情

EQUATION

反应方程式

HRID 220684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Of the compound from Example 168A, 2.4 g (9.24 mmol) were suspended with 2.55 g (18.48 mmol) of potassium carbonate in 48 ml of acetonitrile. Then 1.08 ml (10.17 mmol) of ethyl chloroacetate were added and the mixture was heated under reflux at 80° C. for 4.5 h. A further 113 mg (0.92 mmol) of ethyl chloroacetate were added, with stirring at 80° C. for 2 h. The suspension was filtered through a layer of silica gel, which was washed with ethyl acetate, and the filtrate was concentrated on a rotary evaporator and dried in an HV. This gave 3.24 g (100% of theory) of the title compound.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. filtrationThe suspension was filtered through a layer of silica gel, which
  3. washwas washed with ethyl acetate
  4. concentrationthe filtrate was concentrated on a rotary evaporator
  5. customdried in an HV