HRID262438
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 4 hours
- temperatureThe mixture was cooled at 0°
- filtrationthe amine hydrobromide was filtered off
- customThe filtrate was evaporated
- extractiona solution of the residue in 2 N hydrochloric acid (200 ml) was extracted with ethyl acetate
- extractionextracted with ethyl acetate
- customThe solvents were evaporated