反应详情

To a solution of Example 260B (3.32 g, 8.56 mmol) in dichloromethane (28.5 mL) was added activated powdered 4 Å molecular sieves (9 g), tetrapropylammonium perruthenate (0.150 g, 0.428 mmol) and N-methylmorpholine-N-oxide (1.505 g, 12.85 mmol), and the mixture was stirred overnight at room temperature. The mixture was filtered through a pad of silica, rinsing with ethyl acetate. The filtrate was concentrated and purified by flash chromatography on silica gel (gradient from 0-20% ethyl acetate-heptanes) to give the title compound. MS (ESI+) m/z 385.8 (M+H)+.

1. filtrationThe mixture was filtered through a pad of silica
2. washrinsing with ethyl acetate
3. concentrationThe filtrate was concentrated
4. custompurified by flash chromatography on silica gel (gradient from 0-20% ethyl acetate-heptanes)