反应详情

To a room temperature solution of INTERMEDIATE 5a (250 mg; 0.54 mmol) in dichloromethane (5 mL) were added triethylamine (0.15 mL; 1.08 mmol), DMAP (cat.) and cyclohexane carbonyl chloride (86 μL; 0.64 mmol). The reaction mixture was stirred for 5 hours then more triethylamine (0.08 mL; 0.58 mmol) and DMAP (cat.) were added. The reaction mixture was stirred overnight then more cyclohexane carbonyl chloride (28 μL; 0.21 mmol) was added. The reaction mixture stirred for 5 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 2% methanol in dichloromethane gave the desired product.

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