反应详情

温度

0 °C

To a solution of 6-fluoro-1-(phenylsulfonyl)-3-(1H-pyrazol-4-yl)-1H-indole (Intermediate 5; 1.0 g; 2.93 mmol) in DMF (50 mL) was added NaH (176 mg; 4.4 mmol; 60%) at 0° C. under nitrogen. The reaction mixture was stirred at 0° C. for 1 hour, added 1,2-dibromoethane (0.83 g; 4.4 mmol), warmed to r.t. and stirred overnight. The mixture was poured into ice-water (50 mL) and extracted by EtOAc (50 mL×3). The combined organic layers was washed with brine (100 mL), dried over anhydrous Na2SO4, concentrated, and purified by a silica gel chromatography (petroleum ether/EtOAc=2/1) to afford 0.48 g (37%) of the title compound as a yellow solid.

1. temperaturewarmed to r.t.
2. stirringstirred overnight
3. extractionextracted by EtOAc (50 mL×3)
4. washThe combined organic layers was washed with brine (100 mL)
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated
7. custompurified by a silica gel chromatography (petroleum ether/EtOAc=2/1)