反应详情

To a solution of tert-butyl (3-hydroxycyclohexyl)carbamate (4.40 g, 20.46 mmol) in DCM (250 mL) was added Dess-Martin periodinane (13.0 g, 30.70 mmol) in portions under cooling in an ice bath. The mixture was stirred at room temperature for 2 h. The reaction was diluted with DCM and washed with aqueous sodium carbonate. The separated organic layer was dried over anhydrous sodium sulfate and concentrated. The crude compound was purified by silica gel column chromatography (40% ethyl acetate in petroleum ether) to afford the title compound (4.0 g, 18.78 mmol, 91% yield). MS (ESI) m/z 214.1 [M+H]+.

1. temperatureunder cooling in an ice bath
2. washwashed with aqueous sodium carbonate
3. dry with materialThe separated organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customThe crude compound was purified by silica gel column chromatography (40% ethyl acetate in petroleum ether)