HRID344185

反应详情

EQUATION

反应方程式

HRID 344185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

960 mg (2.5 mmol) of 4'-[(2-n-butyl-benzimidazol-1-yl)-methyl]biphenyl-2-carboxylic acid are dissolved in 25 ml of methylene chloride, treated with 2 ml of thionyl chloride and heated under reflux for one hour. The solvent is then distilled off and evaporated 2 times after adding methylene chloride. 390 mg (2.5 mmol) of benzenesulphonamide are added to the residue and the mixture is heated for one hour at 140° C. After cooling, the oil obtained is taken up in ethyl acetate/sodium chloride solution and extracted 3 times using ethyl acetate. The combined ethyl acetate phases are dried over sodium sulphate, evaporated and the crude product obtained is purified over a silica gel column using methylene chloride/ethanol as eluting agent.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for one hour
  3. distillationThe solvent is then distilled off
  4. customevaporated 2 times
  5. additionafter adding methylene chloride
  6. temperatureAfter cooling
  7. customthe oil obtained
  8. extractionextracted 3 times
  9. dry with materialThe combined ethyl acetate phases are dried over sodium sulphate
  10. customevaporated