反应详情

温度

70 °C

To a solution of 7-aza indazole (250 mg, 2.1 mmol) and ethyl bromoacetate (0.47 mL, 4.2 mmol) in DMF (8 mL) was added K2CO3 (1.16 gm, 8.4 mmol) and the resulting mixture stirred at 70° C. for 16 hours. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (20 mL). The organic layer was washed with water (2×5 mL), brine (5 mL), dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude material was purified using silica gel column chromatography eluting with EtOAc:hexane 10:90 to afford the title compound as an off-white solid in 49% yield, 210 mg.

1. temperatureThe reaction mixture was cooled to room temperature
2. washThe organic layer was washed with water (2×5 mL), brine (5 mL)
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe crude material was purified
7. washeluting with EtOAc:hexane 10:90