反应详情

温度

85 °C

To a solution of ethyl 4-[7-(1-ethylpropyl)-2-oxo-2,3-dihydro-1H-benzimidazol-1-yl]butanoate (9.7 g, 30.5 mmol) and 2,2′-azobisisobutyronitrile (AIBN; 0.5 g, 3.05 mmol) in chlorobenzene (100 mL) was added N-chlorosuccinimide (NCS; 4.35 g, 32.6 mmol) in portions at 65° C., and the mixture was stirred at 80-90° C. for 2 days. After cooled to room temperature, the reaction mixture was partitioned between ethyl acetate (50 mL) and water (50 mL). The aqueous phase was extracted with ethyl acetate (100 ml×3), washed with brine (100 mL), dried over anhydrous sodium sulfate and purified by silica gel column (petroleum ether/ethyl acetate, 50/1) to afford the title compound (6.8 g, 61%) as yellow oil.

1. temperatureAfter cooled to room temperature
2. customthe reaction mixture was partitioned between ethyl acetate (50 mL) and water (50 mL)
3. extractionThe aqueous phase was extracted with ethyl acetate (100 ml×3)
4. washwashed with brine (100 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. custompurified by silica gel column (petroleum ether/ethyl acetate, 50/1)