HRID2164789

反应详情

EQUATION

反应方程式

HRID 2164789 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chlorobenzenesulphonyl chloride (1.56 g) was added in portions over 2 minutes to a solution of 2-amino-N-(3-imidazol-1-ylpropyl)benzamide (1.8 g) in water (50 ml) at 80° C. on a steam bath. The mixture was stirred at 80°-90° C. for 3 hours, cooled to room temperature and brought to pH 7 with saturated aqueous sodium bicarbonate solution. The crude product which had precipitated was extracted into dichloromethane (2×100 ml); the resulting solution was dried over magnesium sulphate and evaporated to give a solid. The solid was recrystallised from ethanol to give 2-(4-chlorobenzenesulphonamido)-N-(3-imidazol-1-ylpropyl)benzamide (1.4 g), in the form of a white solid, m.p. 174°-176° C.

WORKUP

后处理

  1. customThe crude product which had precipitated
  2. extractionwas extracted into dichloromethane (2×100 ml)
  3. dry with materialthe resulting solution was dried over magnesium sulphate
  4. customevaporated
  5. customto give a solid
  6. customThe solid was recrystallised from ethanol