HRID2420116

反应详情

EQUATION

反应方程式

HRID 2420116 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methanesulphonyl chloride (60 parts) in acetone (800 parts) was added dropwise to a suspension of 5,6-dichloro-benzimidazole (94 parts) in acetone (240 parts) containing triethylamine (50 parts). A precipitate of triethylamine hydrochloride was observed and the temperature rose to 40° C. The mixture was heated under reflux for 10 minutes and then stirred at room temperature for 20 hours. On pouring into cold water (4000 parts) a solid product precipitated out, which was filtered off, washed with water, dried and recrystallised from acetone (charcoal) to give 5,6-dichloro-1-(methylsulphonyl)-benzimidazole (61 parts) as pale yellow needles, melting point 191°-193° C.

WORKUP

后处理

  1. customrose to 40° C
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 10 minutes
  4. customprecipitated out
  5. filtrationwhich was filtered off
  6. washwashed with water
  7. customdried
  8. customrecrystallised from acetone (charcoal)