HRID1031499

反应详情

EQUATION

反应方程式

HRID 1031499 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

In dimethyl formamide (10 ml) was suspended 60% sodium hydride (dispersion in paraffin) (288 mg), to which was added dropwise a solution of 2-chlorophenol (926 mg) in dimethylformamide. When exothermic reaction and evolution of hydrogen gas ceased, 2-chloro-5-(3,4-dimethoxybenzoyl)pyridine (1 g) was added to the reaction mixture, followed by stirring for hours at 80° C. The reaction mixture was poured into ice-water, then precipitating substance was collected by filtration, and purified by means of a silica gel column chromatography [eluent: n-hexane+ethyl acetate (1:1)] to obtain 2-(2-chlorophenoxy)-5-(3,4-dimethoxybenzoyl)pyridine (1.1 g) as an oil.

WORKUP

后处理

  1. customprecipitating substance
  2. filtrationwas collected by filtration
  3. custompurified by means of a silica gel column chromatography [eluent: n-hexane+ethyl acetate (1:1)]