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Ethylene Glycol → 2-(2-Methyl[1,3]dioxolane-2-yl)furan
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Acetylfuran | HCID 14505 | — |
| 反応物 | Ethyl orthoformate | HCID 31214 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(2-Methyl[1,3]dioxolane-2-yl)furan | HCID 11744835 | 50% |
反応手順
A mixture of 4 mL (139.6 mmol) 2-acetylfuran, 8.7 mL (156 mmol) of ethylene glycol, 198 mg (1 mmol) of ptoluenesulfonic acid monohydrate, and 22 mL (132.3 mmol) of triethyl orthoformate was reacted at room temperature under N2 for 3 days. The reaction mixture was poured into a mixture of ethyl acetate (100 mL) and water (100 mL). The aqueous layer was extracted with ethyl acetate (3×50 mL), and the combined organic layer was washed with water (100 mL), sodium bicarbonate solution (150 mL), and brine (100 mL). The organic layer was dried over MgSO4, concentrated in vacuo, and the residue was distilled under reduced pressure (1.5 tort) to afford 9.98 g (50%) of 2-(2-methyl-1,3-dioxolan-2-yl)-furan, as a clear oil, b.p. 24° C./1.5 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05514679 |
| 出典データセット | uspto-grants-1996_05 |
| ORD ID | ord-84b3147593fa4b128550e1ee6d74426a |
| 出典メモ | uspto-grants-1996_05 |