反应详情

To a solution of compound 1I (3.3 g, 9.97 mmol) in 10% CH3CN in CH2Cl2 (50 mL) at rt was added NMO (3.0 g, 25.6 mmol) followed by tetrapropyl ammonium perruthenate (300 mg, 0.85 mmol). After a mild exotherm, the reaction was stirred at rt for 4 h. The reaction was diluted with hexane (50 mL), mixed well and filtered through a plug of silica gel (˜50 g). The silica plug was washed liberally with 30% EtOAc in hexane (500 mL). Solvents were removed under vacuum. Purification by flash chromatography (silica gel, 0-15% EtOAc in hexanes) provided the title compound (2.94 g).

1. additionmixed well
2. filtrationfiltered through a plug of silica gel (˜50 g)
3. washThe silica plug was washed liberally with 30% EtOAc in hexane (500 mL)
4. customSolvents were removed under vacuum
5. customPurification by flash chromatography (silica gel, 0-15% EtOAc in hexanes)