反应详情

To a stirred mixture of 6.5 parts of 5-chloro-2-methyl-1H-benzimidazole-1-propanol and 120 parts of trichloromethane are added dropwise 12 parts of sulfinyl chloride. Upon completion, the whole is heated to reflux and stirring is continued for 3 hours at reflux temperature. The reaction mixture is cooled and evaporated. Water is added to the residue and the mixture is treated with activated charcoal. The latter is filtered off and the filtrate is alkalized with ammonium hydroxide. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 5-chloro-1-(3-chloropropyl)-2-methyl-1H-benzimidazole.

1. temperatureUpon completion, the whole is heated
2. temperatureto reflux
3. temperatureat reflux temperature
4. temperatureThe reaction mixture is cooled
5. customevaporated
6. additionWater is added to the residue
7. additionthe mixture is treated with activated charcoal
8. filtrationThe latter is filtered off
9. extractionThe product is extracted with trichloromethane
10. customThe extract is dried
11. filtrationfiltered
12. customevaporated
13. customThe residue is crystallized from 2,2'-oxybispropane
14. filtrationThe product is filtered off
15. customdried