反应详情

A solution of 132d (120 mg, 0.18 mmol) in methanol/dichloromethane (4/4 mL) was added NaBH4 (15 mg, 0.60 mmol). The mixture was stirred at room temperature for 1 h and quenched with water (2 mL). It was then evaporated under reduced pressure and the residue was purified by reverse-phase prep-HPLC to afford 132 (60 mg, 50%) as a white solid. MS-ESI: [M+H]+ 654.3. 1H NMR (500 MHz, MeOD-d4) δ 8.94 (d, J=2.5 Hz, 1H), 8.61 (d, J=5.0 Hz, 1H), 8.51 (d, J=2.5 Hz, 1H), 8.35 (d, J=2.0 Hz, 1H) 7.88 (d, J=1.5 Hz, 1H), 7.75 (d, J=1.5 Hz, 1H), 7.72-7.69 (m, 1H), 7.65 (d, J=5.0 Hz, 1H), 7.61 (d, J=2.5 Hz, 1H), 7.13 (d, J=7.5 Hz, 1H), 4.62-4.58 (m, 2H), 4.36-4.31 (m, 1H), 3.61-3.84 (m, 2H), 3.71-3.67 (m, overlap, 5H), 3.56-3.47 (m, 2H), 1.47 (s, 9H), 1.39 (d, J=7.0 Hz, 3H).

1. customquenched with water (2 mL)
2. customIt was then evaporated under reduced pressure
3. customthe residue was purified by reverse-phase prep-HPLC