HRID269593

反应详情

EQUATION

反应方程式

HRID 269593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

67.2 g (0.48 mol) of potassium carbonate are added to a solution of 100 g (0.40 mol) of 2-hydroxy-5-iodobenzaldehyde (Example 1A) in 1.5 l of dimethylformamide and, after a few minutes, 51 ml (0.44 mol) of benzyl chloride are added. The reaction mixture is stirred under reflux at 120° C. for 24 h. After stirring at RT for a further 24 h and the addition of 1.5 l of water, a solid crystallizes out. The precipitate is collected by suction filtration, washed twice with water and dried in vacuo. The solid is recrystallized from 230 ml of ethanol. 122.9 g (90% of theory) of product are obtained.

WORKUP

后处理

  1. stirringAfter stirring at RT for a further 24 h
  2. customa solid crystallizes out
  3. filtrationThe precipitate is collected by suction filtration
  4. washwashed twice with water
  5. customdried in vacuo
  6. customThe solid is recrystallized from 230 ml of ethanol
  7. custom122.9 g (90% of theory) of product are obtained