反应详情

温度

10 °C

To a solution of 1H-pyrazolo[3,4-c]pyridine (0.50 g, 3.5 mmol) in water (10 mL) was added a solution of sodium oxybromide (prepared by dropwise addition of bromine (0.25 mL) to sodium hydroxide solution (0.40 mg in 5 mL) at 0° C. over 5 min). The reaction mixture stirred for 1 h at 10° C. The mixture was then acidified to pH ˜5.5 with ammonium chloride, and extracted with ethyl acetate (3×20 mL). The combined organic fractions were dried over sodium sulfate and concentrated to afford 0.43 g (62%) of the title compound. 1H NMR (300 MHz, CD3OD): δ 7.79 (dd, J=1.5, 4.2 Hz, 1H), 8.32-8.33 (d, J=5.7 Hz, 1H), 9.07 (s, 1H).

1. extractionextracted with ethyl acetate (3×20 mL)
2. dry with materialThe combined organic fractions were dried over sodium sulfate
3. concentrationconcentrated