反应详情

A solution of Example 155 (500 mg, 1.16 mmol) in anhydrous CH2Cl2 (20 mL) was treated at 0° C. with triflic acid (1741 mg, 11.6 mmol) for 1 h. A saturated solution of sodium bicarbonate was added and the organic layer was separated, dried with anhydrous MgSO4 and concentrated under reduced pressure to afford 400 mg of crude material, which was used directly without purification in the next reactions. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.55-1.71 (m, 9H), 3.77-3.87 (m, 3H), 7.18 (d, J=9.1 Hz, 1H), 7.54 (dd, J=8.9, 2.2 Hz, 1H), 7.81 (d, J=2.4 Hz, 1H), 8.65 (s, 1H); MS (DCI/NH3) m/z 341 (M+H)+.

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