反应详情

To a suspension of hexane-washed NaH (0.72 g, 60%, 18 mmol) in tetrahydrofuran (30 mL) was added a solution of 4,4-dimethylcyclohexanone (2.0 g, 15.6 mmol) in tetrahydrofuran (20 mL). The suspension was stirred at room temperature for 30 minutes. Then dimethylcarbonate (6.31 mL, 75 mmol) was added dropwise by syringe. The mixture was heated to reflux for four hours. The mixture was acidified with 5% HCl and extracted with dichloromethane (100 mL×3) and washed with water, brine, and dried over Na2SO4. After concentration, the crude product was loaded on a column and eluted with 10% ethyl acetate in hexane to give title compound.

1. temperatureThe mixture was heated
2. temperatureto reflux for four hours
3. extractionextracted with dichloromethane (100 mL×3)
4. washwashed with water, brine
5. dry with materialdried over Na2SO4
6. concentrationAfter concentration
7. washeluted with 10% ethyl acetate in hexane