反应详情

The HCl salt from EXAMPLE 1D was dissolved in methanol (500 mL) and 7M ammonia in methanol (13.9 mL, 97 mmol) was added dropwise. The mixture was stirred at room temperature for 10 minutes and concentrated. The residue was washed with water and concentrated to provide the title compound as the free base. MS (ESI) m/e 310 (M+H)+; 1H NMR (DMSO-d6) δ 1.17-1.81 (m, 8H), 1.93-2.07 (m, 2H), 3.71-3.98 (m, 1H), 6.05 (s, 1H), 6.37 (d, J=6.35 Hz, 1H), 7.15 (dd, J=8.13, 4.56 Hz, 1H), 8.19 (d, J=2.78 Hz, 1H), 8.25 (dd, J=4.76, 1.59 Hz, 1H), 8.63 (d, J=7.14 Hz, 1H), 10.17 (s, 1H), 12.11 (s, 1H).

1. concentrationconcentrated
2. washThe residue was washed with water
3. concentrationconcentrated