反应详情

温度

0 °C

An ice cold mixture of 9-1 (43 mg, 0.089 mmol), 4 Å molecular sieves (56 mg) and NMO (16 mg, 0.14 mmol) in dichloromethane (0.5 mL) was treated with TPAP (3 mg, 0.009 mmol). The mixture was stirred for 5 min. at 0° C. and then for 1 h at room temperature. The mixture was then filtered through a pad of silica gel, washing with ethyl acetate. The solvents were evaporated and the residue was purified by flash chromatography on silica gel (10% ethyl acetate/hexanes) to give 9-2 (34 mg, 79%).

1. waitfor 1 h at room temperature
2. filtrationThe mixture was then filtered through a pad of silica gel
3. washwashing with ethyl acetate
4. customThe solvents were evaporated
5. customthe residue was purified by flash chromatography on silica gel (10% ethyl acetate/hexanes)