HRID704566

反应详情

EQUATION

反应方程式

HRID 704566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-(2-aminophenyl)-4-chlorobutan-1-one hydrochloride (b 11.3 g, 0.0427 mol) in concentrated hydrochloric acid (1200 ml) was cooled down to 0° with stirring. Then sodium nitrite (3.54 g, 0.051mol) in water (25 ml) was added dropwise. On completion of the addition, the reaction mixture was allowed to warm to room temperature and stirred overnight. The solution was evaporated under reduced pressure to dryness. The solid obtained was washed with a solution of sodium acetate and collected by filtration to give the title compound, 5.32 g. Recrystallization from methanol gave the product, m.p. 201-203°.

WORKUP

后处理

  1. additionOn completion of the addition
  2. stirringstirred overnight
  3. customThe solution was evaporated under reduced pressure to dryness
  4. customThe solid obtained
  5. washwas washed with a solution of sodium acetate
  6. filtrationcollected by filtration