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
To a stirred mixture of 45 parts of 5-chloro-2-(phenylmethyl)-1H-benzimidazole-1-propanol and 225 parts of trichloromethane are added dropwise 29.75 parts of sulfinyl chloride. Upon completion, stirring is continued for 6 hours at reflux temperature. The reaction mixture is evaporated and the residue is taken up in water. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The reisude is purified by columnchromatography over silica gel using a mixture of trichloromethane and methanol (98:2) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 5-chloro-1-(3-chloropropyl)-2-(phenylmethyl)-1H-benzimidazole as a solid residue.
WORKUP
后处理
- temperatureat reflux temperature
- customThe reaction mixture is evaporated
- extractionThe product is extracted with trichloromethane
- customThe extract is dried
- filtrationfiltered
- customevaporated
- customThe reisude is purified by columnchromatography over silica gel using
- additiona mixture of trichloromethane and methanol (98:2) as eluent
- customThe pure fractions are collected
- customthe eluent is evaporated