HRID46489

反应详情

EQUATION

反应方程式

HRID 46489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of sodium nitrite (2.38 g) in water (10 ml) was added dropwise to a mixture of 3-amino-2-hydroxymethylpyridine (4.8 g), aqueous hydrochloric acid (48%, 10 ml) and water (5 ml) stirred at 0°-5°. This solution was added to a hot solution of cuprous chloride (2.5 g) in conc. hydrochloric acid and the mixture was heated on a steam-bath for 0.5 hours, diluted with water and saturated with hydrogen sulphide. The mixture was filtered, concentrated and extracted with chloroform and the chloroform extract was evaporated to give 3-chloro-2-hydroxymethylpyridine (3.7 g) m.p. 42°-44° (from n-pentane).

WORKUP

后处理

  1. temperaturethe mixture was heated on a steam-bath for 0.5 hours
  2. filtrationThe mixture was filtered
  3. concentrationconcentrated
  4. extractionextracted with chloroform
  5. extractionthe chloroform extract
  6. customwas evaporated