反应详情

A solution of compound 118 (3.9 g, 12.986 mmol) in acetone (50 mL) was treated with 10% aq. HCl (50 mL) at room temperature and stirred for over night (14 h). Solvent was evaporated and crude was basified using 10% aq. NH4OH solution (100 mL). The solid was filtered off, washed with 10% NH4OH solution (20 mL), water (2×15 mL) and dried under vacuum to obtain compound 119 (2.81 g, 85%) as a yellow solid. mp 175-177° C.; 1H NMR (DMSO-d6) δ 2.58 (t, 2H, J=6.9 Hz), 2.90 (t, 2H, J=6.9 Hz), 3.04-3.10 (m, 2H), 6.24 (t, 1H, J=3.9 Hz), 7.90-8.01 (m, 3H), 8.33 (d, 1H, J=2.1 Hz), 11.95 (s, 1H); ESI-MS (m/z, %): 279 (M+Na, 100), 257 (MH+, 33).

1. customSolvent was evaporated
2. filtrationThe solid was filtered off
3. washwashed with 10% NH4OH solution (20 mL), water (2×15 mL)
4. customdried under vacuum