HRID582768

反应详情

EQUATION

反应方程式

HRID 582768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 0.38 g of NaNO2 in 4.5 ml of water is added slowly to a solution, cooled to -5° C., of 0.95 g of the product obtained in step C in 22 ml of concentrated HCl and 21 ml of AcOH, and the mixture is stirred for 1 h 15 min at 0° C. It is cooled to -10° C., and a solution of 3.76 g of SnCl2.2H2O in 8 ml of concentrated HCl is added slowly. After 4 hours of stirring at RT, the mixture is filtered, and the residue is washed with 2 ml of concentrated HCl and dried under vacuum to obtain 1 g of expected product.

WORKUP

后处理

  1. temperatureIt is cooled to -10° C.
  2. stirringAfter 4 hours of stirring at RT
  3. filtrationthe mixture is filtered
  4. washthe residue is washed with 2 ml of concentrated HCl
  5. customdried under vacuum