反应详情

A mixture of 199e (1.24 g, 3.2 mmol), HCHO solution (15 mL, 37% in water), acetic acid (1 mL) and NaBH(OAc)3 (1.36 g, 6.4 mmol) in methanol (10 mL) was stirred at room temperature for 4 h. The solvent was evaporated in vacuo and the residue was extracted with ethyl acetate (20 mL×3). The combined extracts were dried over sodium sulfate and concentrated under reduced pressure. The residue was purified on reverse phase Combi-flash to give 199f (940 mg, 80%). MS: [M+H]+ 365.

1. customThe solvent was evaporated in vacuo
2. extractionthe residue was extracted with ethyl acetate (20 mL×3)
3. dry with materialThe combined extracts were dried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified on reverse phase Combi-flash