反应详情

温度

65 °C

A mixture of ethyl 2-mercaptobenzimidazole-5-carboxylate (1.29 g), anhydrous potassium carbonate (960 mg) in N,N-dimethylformamide (20 ml) was stirred at 60-70 ° C. for 30 minutes. To this mixture was added a solution of 4-(4-acetyl-3-hydroxy-2-propylphenylthio)butylbromide (2.00 g) in N,N-dimethylformamide (10 ml) dropwise during 10 minutes and stirred at the same temperature for 30 minutes. The reaction mixture was poured into ice-water, made acidic with concentrated hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous sodium sulfate and evaporated. The resulting residue was purified by silica gel column chromatography, eluting with dichloromethane-ethyl acetate 10:1), to give the title compound (2.53 g, 89.8%) as pale yellow oil.

1. stirringstirred at the same temperature for 30 minutes
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customevaporated
6. customThe resulting residue was purified by silica gel column chromatography
7. washeluting with dichloromethane-ethyl acetate 10:1),