反应详情

Hydroxylamine hydrochloride (1.5 g) and potassium carbonate (3.83 g) were stirred together in absolute ethanol (100 ml) for 15 minutes. Indazole-3-carbonitrile (2 g) was added and the solution heated at reflux for 4 hours, cooled to room temperature and diluted with methanol (5 ml). The solution was filtered and the solvent evaporated. The residue was extraced with anhydrous either, the extracts were dried over MgSO4, filtered and the solvent removed to afford a white solid, which was recrystallised from acetone/dichloromethane to afford the title compound (900 mg), m.p. 155°-158° C. δH (360 MHz, CDCl3) 6.46 (1 H, brm, N--OH), 7.17 (1 H, t, J=1 Hz, H-6), 7.41 (1 H, t, J=2 Hz, H-5), 7.55 (1 H, d, J=2 Hz, H-4), 8.03 (1 H, t, J=2 Hz, H-7 ); m/z (M+, 100%), 176 (100), 144 (80), 119 (25), 92 (15).

1. temperaturethe solution heated
2. temperatureat reflux for 4 hours
3. filtrationThe solution was filtered
4. customthe solvent evaporated
5. dry with materialwere dried over MgSO4
6. filtrationfiltered
7. customthe solvent removed
8. customto afford a white solid, which
9. customwas recrystallised from acetone/dichloromethane