反应详情

To a solution of 4 (6.75 g, 31.38 mmol) in dry THF (200 mL) at 0° C. under nitrogen atmosphere BH3.THF solution (82 mL, 1 M in THF) was added dropwise. The mixture was allowed to warm to room temperature and stirred for 1 h. The reaction was quenched with 6N ice-cold aq. HCl (30 mL), made alkaline (pH 7-8) with 2 N NaOH, saturated with NaCl, extracted with EtOAc, the extracts were dried (MgSO4), concentrated. Purification by chromatoghraphy on silica gel using CH2Cl2 as eluent afforded (3.95 g, 68% yield) as an off white solid. 1H NMR (300 MHz, MeOH-d4): δ 7.87 (m, 1H), 7.51 (dd, 8.5, 0.8 Hz, 1H), 7.47 (d, 8.5 Hz, 1H), 7.37 (d, 3.2 Hz, 1H), 7.34 (dd, 8.5, 1.6 Hz, 1H), 6.57 (dd, 3.2, 0.8 Hz, 1H). MS m/z: 184 (M−1).

1. customThe reaction was quenched with 6N ice-cold aq. HCl (30 mL)
2. extractionsaturated with NaCl, extracted with EtOAc
3. dry with materialthe extracts were dried (MgSO4)
4. concentrationconcentrated
5. customPurification by chromatoghraphy on silica gel
6. customafforded (3.95 g, 68% yield) as an off white solid