反应详情

To a room temperature solution of INTERMEDIATE 5a (300 mg; 0.64 mmol) in 1,2-dichloroethane (15 mL) were added cyclohexanone (0.20 mL; 1.93 mmol), sodium triacetoxy borohydride (0.43 g; 2.05 mmol) and acetic acid (37 μL; 0.64 mmol). The reaction mixture was stirred for 6 hours then was washed with two portions of saturated sodium bicarbonate. The organic phase was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. Column chromatography eluting with 4% methanol in dichloromethane gave the desired product.

1. washthen was washed with two portions of saturated sodium bicarbonate
2. dry with materialThe organic phase was dried over anhydrous sodium sulphate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. washColumn chromatography eluting with 4% methanol in dichloromethane