反应详情

To a stirred solution of compound (50) (0.50 g, 1.3 mmol) in dichloromethane (15 mL) was added pyridinium chlorochromate (0.55 g, 2.6 mmol) followed by NaOAc (0.21 g, 2.57 mmol) at room temperature. The resulting reaction was stirred overnight at room temperature (monitored by LC/MS), then filtered. The solid was washed with dichloromethane (2×25 mL) and the combined filtrates were washed with water (2×25 mL), dried over MgSO4 and concentrated in vacuo to provide compound 51 which was used in the next step without further purification. MS (ESI): m/z=388.38 (M+H+).

1. customThe resulting reaction
2. filtrationfiltered
3. washThe solid was washed with dichloromethane (2×25 mL)
4. washthe combined filtrates were washed with water (2×25 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo