反应详情

To a 0° C. cold solution of 2.00 g (10.8 mmol) of (3-oxo-cyclobutyl)-carbamic acid tert-butyl ester in 20 mL of ethanol was added portionwise 204 mg (5.40 mmol) of sodium borohydride. The reaction mixture was stirred at room temperature until complete conversion was achieved. The solvent was evaporated, the crude product was taken up in dichloromethane and treated with sat. sodium bicarbonate solution. The phases were separated and the aqueous phase extracted twice with dichloromethane. The organic phases were combined, dried over magnesium sulfate and concentrated to give crude (3-hydroxy-cyclobutyl)-carbamic acid tert-butyl ester. Rt=0.76 min (Method C). Detected mass: 132.2 (M-tBu+H+).

1. customThe solvent was evaporated
2. additiontreated with sat. sodium bicarbonate solution
3. customThe phases were separated
4. extractionthe aqueous phase extracted twice with dichloromethane
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated