関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-Bromofuran-2-carboxylic acid | HCID 605479 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Ethyl 3-bromofuran-2-carboxylate | HCID 22456149 | 54.3% |
反応手順
3-Bromofuran-2-carboxylic acid (1.86 g, 9.75 mmol), ethyl iodide (3.1 mL, 38.8 mol) and cesium carbonate (4.80 g, 14.7 mmol) were suspended in acetonitrile (50 mL), followed by stirring at 80° C. for 3 hours. Aqueous saturated sodium hydrogencarbonate solution was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was distilled away under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane:ethyl acetate=9:1) to afford ethyl 3-bromofuran-2-carboxylate (1.16 g, 54%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889718B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-a3b9f2d876214edcbe0ca512f91496f6 |
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| 出典メモ | uspto-grants-2014_11 |
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