反应详情

温度

95 °C

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 1-furan-2-yl-ethanone (50.00 g, 454.0 mmol) in ethylene glycol (500.0 mL) was treated with trimethylorthoformate (100.0 mL, 908.0 mmol) followed by LiBF4 (7.00 g, 75 mmol). The reaction mixture was heated at 95° C. overnight. Sat. aq. NaHCO3 (500 mL) was added and the mixture was extracted with EA (500 mL). The org. extracts were washed with brine (2×250 mL), dried over MgSO4, filtered, and the solvent was removed under reduced pressure. Purification of the residue by distillation (11 mbar, 71-73° C.) gave the title compound as a colorless oil.

1. extractionthe mixture was extracted with EA (500 mL)
2. washextracts were washed with brine (2×250 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customthe solvent was removed under reduced pressure
6. customPurification of the residue
7. distillationby distillation (11 mbar, 71-73° C.)