HRID2164790

反应详情

EQUATION

反应方程式

HRID 2164790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(4-Chlorobenzenesulphonamido)benzoyl chloride (3.40 g) was added in portions to a stirred mixture of 3-imidazol-1-ylpropylamine (1.29 g), triethylamine (1.04 g) and dimethylformamide (25 ml) at room temperature. The temperature of the mixture rose to 33° C.; the mixture was then stirred at room temperature for 4 hours before pouring into water (500 ml). The aqueous solution was decanted from the crude product which had precipitated as a gum. This gummy material was dissolved in dichloromethane (50 ml), the solution was dried over magnesium sulphate and the solution was evaporated. The crude product was recrystallised from ethyl acetate to give 2-(4-chlorobenzenesulphonamido)-N-(3-imidazol-1-ylpropyl)benzamide, in the form of a white solid, m.p. 175°-177° C. (yield: 2.1 g).

WORKUP

后处理

  1. customrose to 33° C.
  2. customThe aqueous solution was decanted from the crude product which
  3. customhad precipitated as a gum
  4. dissolutionThis gummy material was dissolved in dichloromethane (50 ml)
  5. dry with materialthe solution was dried over magnesium sulphate
  6. customthe solution was evaporated
  7. customThe crude product was recrystallised from ethyl acetate