反应详情

温度

25 °C

A mixture of 330a (1.0 g, 2.76 mmol), triethylamine (610 mg, 6.0 mmol), and acetic anhydride (5 mL) was stirred at 25° C. for 2 h. Then the reaction mixture was quenched with water (10 mL) and the pH was adjusted to around 8 with NaHCO3 (aq.). The mixture was extracted with dichloromethane (2×15 mL). The combined dichloromethane extract was concentrated under reduced pressure and the residue was purified by silica-gel column chromatography eluting with 1:1 ethyl acetate/petroleum ether to afford 330b as a pale yellow solid (1.0 g, 90%). MS-ESI: [M+H]+ 405.2

1. customThen the reaction mixture was quenched with water (10 mL)
2. extractionThe mixture was extracted with dichloromethane (2×15 mL)
3. extractionThe combined dichloromethane extract
4. concentrationwas concentrated under reduced pressure
5. customthe residue was purified by silica-gel column chromatography
6. washeluting with 1:1 ethyl acetate/petroleum ether