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A mixture of alcohol 266 (2.75 g, 10.45 mmol), NMO (5.8 g, 49 mmol) and 4 Å molecular sieves (8.34 g) was suspended in dry DCM (100 mL) and dry 1,2-dichloroethane (100 mL), stirred at room temperature for 45 min, and then cooled to 0° C. for the addition of solid TPAP (0.36 g, 1.03 mmol). The reaction mixture was stirred at 0° C. for 30 min and then at room temperature for 5 h, filtered through Celite®/silica gel using 50% AcOEt in hexanes as an eluent, then concentrated. The residue was purified by flash chromatography (eluent: 30% to 50% AcOEt in hexane) to provide title compound 267 (0.78 g, 29% yield).

1. waitat room temperature for 5 h
2. filtrationfiltered through Celite®/silica gel using 50% AcOEt in hexanes as an eluent
3. concentrationconcentrated
4. customThe residue was purified by flash chromatography (eluent: 30% to 50% AcOEt in hexane)