HRID262438

反应详情

EQUATION

反应方程式

HRID 262438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-bromo-1-[4-hydroxy-3-(hydroxymethyl)phenyl]ethanone (9.1 g) and N-methyl-N-phenyl-N'-(phenylmethyl)-1,3-benzenediamine (16.6 g) in butanone (200 ml) was heated under reflux for 4 hours. The mixture was cooled at 0° and the amine hydrobromide was filtered off. The filtrate was evaporated and a solution of the residue in 2 N hydrochloric acid (200 ml) was extracted with ethyl acetate. The acidic solution was basified with solid sodium bicarbonate and then extracted with ethyl acetate. The solvents were evaporated to give a brown gum (10.7 g). The crude product in ethyl acetate was filtered through a column of silica (100 g) to yield a light brown gum (7.9 g).

WORKUP

后处理

  1. temperatureunder reflux for 4 hours
  2. temperatureThe mixture was cooled at 0°
  3. filtrationthe amine hydrobromide was filtered off
  4. customThe filtrate was evaporated
  5. extractiona solution of the residue in 2 N hydrochloric acid (200 ml) was extracted with ethyl acetate
  6. extractionextracted with ethyl acetate
  7. customThe solvents were evaporated