反应详情

A solution of chlorosulfuric acid in 20 ml of carbon tetrachloride was added under ice cooling to a solution of 11.18 g of imidazo[5,1-b]thiazole in 200 ml of carbon tetrachloride. The reaction mixture was heated under reflux for 6 hr. Water was added thereto under ice cooling to terminate the reaction. The mixture was extracted with dichloromethane. The organic layers were combined together. The combined organic layers were washed with a dilute aqueous sodium hydroxide solution and saturated brine in that order and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation. Isopropyl ether was added to the residue. The resultant powder was collected by filtration to give 4.01 g of 7-chlorosulfonylimidazo[5,1-b]thiazole.

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 6 hr
3. customunder ice cooling to terminate
4. customthe reaction
5. extractionThe mixture was extracted with dichloromethane
6. washThe combined organic layers were washed with a dilute aqueous sodium hydroxide solution and saturated brine in that order
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was removed by distillation
9. additionIsopropyl ether was added to the residue
10. filtrationThe resultant powder was collected by filtration