反応 #71023

反応方程式

1-furan-2-yl-ethanone

trimethylorthoformate

N2

NaHCO3

→

title compound

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

溶媒

ethylene glycol

反応条件

後処理

1. 1
   抽出the mixture was extracted with EA (500 mL)
2. 2
   洗浄extracts were washed with brine (2×250 mL)
3. 3
   乾燥dried over MgSO4
4. 4
   ろ過filtered
5. 5
   その他the solvent was removed under reduced pressure
6. 6
   その他Purification of the residue
7. 7
   workup.DISTILLATIONby distillation (11 mbar, 71-73° C.)

実験手順

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.

出典