반응 #71023

반응 방정식

1-furan-2-yl-ethanone

trimethylorthoformate

N2

NaHCO3

→

title compound

2-Furan-2-yl-2-methyl-[1,3]dioxolane

용매

ethylene glycol

반응 조건

후처리

1. 1
   추출the mixture was extracted with EA (500 mL)
2. 2
   세척extracts were washed with brine (2×250 mL)
3. 3
   건조dried over MgSO4
4. 4
   여과filtered
5. 5
   기타the solvent was removed under reduced pressure
6. 6
   기타Purification of the residue
7. 7
   workup.DISTILLATIONby distillation (11 mbar, 71-73° C.)

실험 절차

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.

출처