反应详情

2-Fluoro-3-oxopentanoic acid methyl ester (2.21 g, 14.9 mmol), ethylene glycol (4.15 mL, 74.5 mmol), and BF3.Et2O (0.189 mL, 1.49 mmol) were mixed in cyclohexane (10 mL). The mixture was heated to reflux for 5 h, and allowed to cool to rt. The mixture was diluted with EtOAc, and washed with brine, water, aq. sat. NaHCO3, and brine again. The org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. The title compound was obtained as an oil (1.88 g, 52%).

1. temperatureThe mixture was heated
2. temperatureto reflux for 5 h
3. washwashed with brine, water, aq. sat. NaHCO3, and brine again
4. dry with materialextracts were dried over MgSO4
5. filtrationfiltered
6. customthe solvents were removed under reduced pressure