反应详情

To a solution of Example 6C (212 mg, 0.534 mmol) in CH2Cl2 (20 mL) at 0° C. was added IM BBr3 in CH2Cl2 (1.6 mL, 1.6 mmol) and the reaction was allowed to warm to room temperature for 3 h. Saturated sodium bicarbonate was added, and the organic layer was separated, washed with brine, dried with anhydrous MgSO4 and concentrated under reduced pressure to provide quantitatively of the title compound. 1H NMR (300 MHz-DMSO-d6) δ: 0.95 (t, J=7 Hz, 4H), 1.37 (s+m, 11H), 1.82 (m, 2H), 4.30 (t, J=7 Hz, 2H), 6.95 (d, J=9 Hz, 1H), 7.40 (d-d, J=9 Hz, 3 Hz, 1H), 7.80 (s, 1H), 8.37 (d, J=3 Hz, 1H), 13.62 (s, 1H); MS (DCI/NH3) m/z 383 (M+H)+.

1. customthe organic layer was separated
2. washwashed with brine
3. dry with materialdried with anhydrous MgSO4
4. concentrationconcentrated under reduced pressure