関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Trimethyl orthoformate | HCID 9005 | — |
| 反応物 | 2-Acetylfuran | HCID 14505 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 生成物 | 2-(2-Methyl[1,3]dioxolane-2-yl)furan | HCID 11744835 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536209B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-2c8f0b2cbdf5456fa3f70c2d09e31f41 |
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| 出典メモ | uspto-grants-2013_09 |
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