HRID2420116
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customrose to 40° C
- temperatureThe mixture was heated
- temperatureunder reflux for 10 minutes
- customprecipitated out
- filtrationwhich was filtered off
- washwashed with water
- customdried
- customrecrystallised from acetone (charcoal)