反应详情

To a solution of compound 28c (example 10, scheme 8) (115 mg, 0.21 mmol) in DCM (10 mL) at −40° C. was added BBr3 (1.0M, 0.86 mL, 0.86 mmol). The reaction mixture was allowed to stir for 1 hr then diluted with MeOH (2 mL) and water (1 mL) and concentrated. The residue was purified by preparative HPLC (Thermo C-18 column, gradient MeOH/water from 95:5 to 60:40) to afford title compound 115 (30 mg, 27% yield) as a white solid. 1H NMR (DMSO-d6). δ (ppm): 10.57 (s, 1H), 9.88 (s, 1H), 9.59 (s, 1H), 8.49 (d, J=5.4 Hz, 1H), 7.92 (dd, J=8.0 Hz, J=1.5 Hz, 1H), 7.86 (dd, J=12.7 Hz, J=2.1 Hz, 1H), 7.85 (s, 1H), 7.76 (s, 1H), 7.48 (t, J=8.8 Hz, 1H), 7.42 (dd, J=9.0 Hz, J=1.7 Hz, 1H), 7.40 (s, 1H), 6.93-6.84 (m, 2H), 6.75 (t, J=8.0 Hz, 1H), 6.63 (d, J=5.5 Hz, 1H), 3.88 (s, 3H), 3.61 (s, 2H). MS (m/z): 518.1 (M+H).

1. concentrationconcentrated
2. customThe residue was purified by preparative HPLC (Thermo C-18 column, gradient MeOH/water from 95:5 to 60:40)