反应 #74767

反应方程式

hydrochloric acid

sodium nitrite

3-amino-2-hydroxymethylpyridine

hydrochloric acid

→

3-chloro-2-hydroxymethylpyridine

溶剂

water

hydrogen sulphide

water

water

反应条件

后处理

1. 1
   温度the mixture was heated on a steam-bath for 0.5 hours
2. 2
   过滤The mixture was filtered
3. 3
   浓缩concentrated
4. 4
   萃取extracted with chloroform
5. 5
   萃取the chloroform extract
6. 6
   其他was evaporated

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).

来源