HRID1441020

反应详情

EQUATION

反应方程式

HRID 1441020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-15 °C

PROCEDURE

实验过程

A solution of 1.9 g of sodium nitrite in 10 ml of water is added to a suspension, cooled to -5° C., of 5.2 g of 4-nitro-1-naphthylamine in 150 ml of concentrated HCl, 100 ml of 1N HCl and 150 ml of AcOH. The mixture is left stirring for 1 hour 15 minutes at a temperature of between -5° C. and 0° C. It is cooled to -15° C., and a solution of 12.5 g of stannous chloride dihydrate in 30 ml of concentrated HCl is added very slowly. The temperature is allowed to rise to RT and the reaction mixture is kept stirring for 2 hours 30 minutes. It is filtered, the solid is then taken up with water and the mixture is filtered again. 5.9 g of the expected product are obtained.

WORKUP

后处理

  1. waitThe mixture is left
  2. customto rise to RT
  3. stirringthe reaction mixture is kept stirring for 2 hours 30 minutes
  4. filtrationIt is filtered
  5. filtrationthe mixture is filtered again