HRID1074857

反应详情

EQUATION

反应方程式

HRID 1074857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.1 g (0.10 mol) of γ-chlorobutyryl chloride in 50 ml of chloroform are added dropwise in the course of 1 hour, at 10°-15° C., to a solution of 17.7 g (0.10 mol) of 1,3-diamino-4,6-dichlorobenzene and 8.7 g (0.11 mol) of pyridine in 500 ml of chloroform. The mixture is then stirred for 2 hours at room temperature, the solution is washed with water and filtered through 40 g of silica gel and the filtrate is concentrated. The resulting product is recrystallised from hexane/toluene. Yield: 13.5 g; melting point 125°-128° C.

WORKUP

后处理

  1. washthe solution is washed with water
  2. filtrationfiltered through 40 g of silica gel
  3. concentrationthe filtrate is concentrated
  4. customThe resulting product is recrystallised from hexane/toluene