反应详情

温度

110 °C

3-[(dimethylamino)sulfonyl]benzoyl chloride (1.97 g) was added to a mixture of 1-(3,5-difluorophenyl)-2-(1,3-dihydro-2H-benzimidazol-2-ylidene)ethanone (865 mg), triethylamine (1.6 mL) and 2-methoxyethyl ether (10 mL), followed by heating with stirring at 110° C. for 30 minutes. Water (0.06 mL) was added, followed by further heating under reflux for 30 minutes. After cooling, water was added, followed by extraction with ethyl acetate. The organic layer was washed with water, concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=1/1), and recrystallized from ethyl acetate/n-hexane to obtain 3-[3-(3,5-difluorophenyl)-2-(1,3-dihydro-2H-benzimidazol-2-ylidene)-3-oxopropanoyl]-N,N-dimethylbenzenesulfonamide (391 mg).

1. temperatureby heating
2. temperatureby further heating
3. temperatureunder reflux for 30 minutes
4. temperatureAfter cooling
5. extractionfollowed by extraction with ethyl acetate
6. washThe organic layer was washed with water
7. concentrationconcentrated under reduced pressure
8. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=1/1)
9. customrecrystallized from ethyl acetate/n-hexane