反应详情

A mixture of 206e (1.24 g, 3.2 mmol), 37% aqueous formaldehyde solution (15 mL), 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 (3×20 mL). The combined extract was dried over sodium sulfate and concentrated under reduced pressure. The residue was purified on reverse-phase Combiflash to afford 206f (940 mg, 80%). MS-ESI: [M+H]+ 365.

1. customThe solvent was evaporated in vacuo
2. extractionthe residue was extracted with ethyl acetate (3×20 mL)
3. extractionThe combined extract
4. dry with materialwas dried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified on reverse-phase Combiflash