反应详情

To a suspension of 1.2 g of 2-mercaptobenzimidazole in 30 ml of ethanol was added 580 mg of potassium hydroxide under stirring and stirred at room termperature for 10 minutes. To this solution was added 2.8 g of 3-(4-acetyl-3-hydroxy-2-propylphenoxy)propylbromide at one time, and stirred at room temperature for 4 hours. The solvent was distilled off under reduced pressure and resulting residue was diluted with dichloromethane-water, then extracted with dichloromethane three times. The organic layer was combined, then washed with water saturated with sodium chloride and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, the resulting residue was recrystallized from dichloromethane-n-hexane to give 2.5 g (yield 81%) of the aimed compound as colorless powder. mp 149°-150° C.

1. stirringstirred at room termperature for 10 minutes
2. stirringstirred at room temperature for 4 hours
3. distillationThe solvent was distilled off under reduced pressure
4. customresulting residue
5. extractionextracted with dichloromethane three times
6. washwashed with water saturated with sodium chloride
7. dry with materialdried over anhydrous sodium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. customthe resulting residue was recrystallized from dichloromethane-n-hexane