Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Nitrogen | HCID 947 | — |
| Edukt | Trimethyl orthoformate | HCID 9005 | — |
| Edukt | 2-Acetylfuran | HCID 14505 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Lösungsmittel | Ethylene Glycol | HCID 174 | — |
| Produkt | 2-(2-Methyl[1,3]dioxolane-2-yl)furan | HCID 11744835 | — |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08536209B2 |
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| Quelldatensatz | uspto-grants-2013_09 |
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| ORD ID | ord-2c8f0b2cbdf5456fa3f70c2d09e31f41 |
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| Quellennotiz | uspto-grants-2013_09 |
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