反应详情

To the product of Example 10h (167.3 mg, 0.57 mmol) in dichloromethane (10 mL) at room temperature was added sodium bicarbonate (50 mg) and Dess-Martin periodinane (365 mg, 0.85 mmol) and the reaction was stirred at room temperature overnight. The mixture was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to afford the title compound as a colorless oil (130 mg, Yield: 78%). 1H NMR (400 MHz, CDCl3) δ 9.32 (s, 1H), 8.61 (d, J=6.0 Hz, 1H), 8.09 (s, 1H), 8.02 (d, J=8.4 Hz, 1H), 7.91 (d, J=8.4 Hz, 1H), 7.73 (d, J=6.0 Hz, 1H), 5.91 (s, 1H), 1.66-1.59 (m, 4H), 1.31 (s, 6H), 1.07 (s, 6H) ppm.

1. concentrationThe mixture was concentrated under reduced pressure
2. customthe residue was purified by silica gel column chromatography