HRID1940170

反应详情

EQUATION

反应方程式

HRID 1940170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

2-Amino-3',4,4',5-tetramethoxybenzophenone hydrochloride (36.0 g) and ethyl 4-chloroacetoacetate (21.4 g) were stirred in ethanol (350 ml) under reflux for 7 hours. After completion of the reaction, triethylamine (10.6 g) was added dropwise at a temperature not over 20° C. and the mixture was stirred at 5° C. for 1 hour. The crystals were collected by filtration, washed twice with 50 ml each of ethanol and dried under reduced pressure to provide ethyl 2-chloromethyl-4-(3,4-dimethoxyphenyl)-6,7-dimethoxyquinoline-3-carboxylate (41.0 g; yield 92%).

WORKUP

后处理

  1. temperatureunder reflux for 7 hours
  2. additionwas added dropwise at a temperature not over 20° C.
  3. filtrationThe crystals were collected by filtration
  4. washwashed twice with 50 ml each of ethanol
  5. customdried under reduced pressure