HRID1283402

反应详情

EQUATION

反应方程式

HRID 1283402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-(3-amino-4-methoxybenzoyl) propionic acid (5 g.) in concentrated hydrochloric acid (25 ml.) was diazotised at 0°C by the addition of a solution of sodium nitrite (1.54 g.) in water (5 ml.). This diazo solution was added with stirring to a solution containing hydrated copper sulphate (6.3 g.) and sodium chloride (5.4 g.) in water (20 ml.) to which had been added a solution containing sodium metabisulphite (1.4 g.) and sodium hyroxide (0.9 g.) in water (10 ml.). The mixture was then heated on the steam bath for 30 minutes when a solid separated. The mixture was cooled, the solid collected and washed with cold water. It was crystallised from methanol to yield the product (4.2 g.), m.p. 187°-189°C.

WORKUP

后处理

  1. additionhad been added a solution
  2. temperatureThe mixture was then heated on the steam bath for 30 minutes when a solid
  3. customseparated
  4. temperatureThe mixture was cooled
  5. customthe solid collected
  6. washwashed with cold water
  7. customIt was crystallised from methanol
  8. customto yield the product (4.2 g.), m.p. 187°-189°C.