反应 #4479

反应方程式

tin

hydrochloric acid

3-methoxyaniline

hydrochloric acid

sodium nitrite

→

title compound

(3-methoxyphenyl)hydrazine hydrochloride

溶剂

water

反应条件

后处理

1. 1
   其他at ca. 0°
2. 2
   其他the temperature below 0° C
3. 3
   workup.STIRRINGThe suspension was stirred for a further 30 min
4. 4
   过滤filtered
5. 5
   洗涤washed with dried ether

实验过程

A suspension of 3-methoxyaniline (10 g) in concentrated hydrochloric acid (85 ml) was stirred at ca. 0° and a solution of sodium nitrite (5.75 g) in water (25 ml) was slowly added over a period of 30 min keeping the temperature of the mixture at ca. 0°. After 1 h a solution of tin II chloride dihydrate (59 g) in concentrated hydrochloric acid (50 ml) was added over a period of 1.5 h, to the cooled suspension keeping the temperature below 0° C. The suspension was stirred for a further 30 min, filtered and washed with dried ether to give the title compound as a solid (14 g) m.p. 171°.

来源