反应详情

14.0 g of the compound obtained in Example 1 was dissolved in CHCl3 (80 mL)-MeOH (20 mL), to which was added 4 N HCl/EtOAc (15 mL), and the resulting mixture was concentrated. The residue was dissolved in 30 mL of MeOH, and 50 mL of water was added to it at 0° C., stirred at room temperature for 18 hours. The resulting precipitate was taken out through filtration, washed with 30% MeOHaq and dried in vacuum to obtain the intended compound. 1H-NMR (300 MHz, DMSO-d6) δ: 10.04 (1H, s), 8.24 (1H, d, J=8.5 Hz), 8.09 (1H, d, J=8.3 Hz), 8.01 (1H, d, J=2.7 Hz), 7.96-7.89 (1H, m), 7.77-7.69 (2H, m), 7.38 (1H, s), 7.06 (1H, d, J=8.9 Hz), 4.37-4.26 (1H, m), 4.18 (3H, s), 3.60-3.39 (2H, m), 3.37-3.22 (1H, m), 2.88 (2H, s), 2.13-1.98 (1H, m), 2.02 (3H, s), 1.94-1.75 (3H, m). MS [M+H]+=460.

1. concentrationthe resulting mixture was concentrated
2. dissolutionThe residue was dissolved in 30 mL of MeOH
3. addition50 mL of water was added to it at 0° C.
4. filtrationThe resulting precipitate was taken out through filtration
5. washwashed with 30% MeOHaq
6. customdried in vacuum
7. customto obtain the intended compound