反应详情

A solution of 5 (200 mg, 1.00 mmol), 1 (161 mg, 1.00 mmol), and acetic acid (300 mg, 5.00 mmol) in methanol (2 mL) was treated with sodium cyanoborohydride (66 mg, 1.05 mmol) at room temperature. The resulting mixture was stirred at room temperature overnight. The solvent was removed in vacuo and the residue dissolved in dichloromethane and sodium bicarbonate solution. The aqueous layer was extracted with three additional portions of dichloromethane and the combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. PCTLC (SiO2, 4 mm, 10% EtOH-90% CHCl3) afforded the title compound (12).

1. customThe solvent was removed in vacuo
2. dissolutionthe residue dissolved in dichloromethane
3. extractionThe aqueous layer was extracted with three additional portions of dichloromethane
4. washthe combined organic extracts were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure