関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 2-(2-Acetyl-4-fluorophenoxy)acetic acid | HCID 11658552 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 5-Fluoro-3-methylbenzofuran | HCID 11679847 | 81% |
反応手順
(2-Acetyl-4-fluoro-phenoxy)-acetic acid (1.87 gm, 8.8 mmol) is dissolved in acetic anhydride (60 mL) and treated with sodium acetate (10 gm, 0.12 mol). The resulting mixture is heated to 110° C. for 5 hr, then cooled to 0° C. H2O (100 mL) is added and the solution is stirred overnight at room temperature. The aqueous solution is then extracted into Et2O (2×75 mL). The combined organic extracts are washed with 3% aqueous KOH (2×75 mL), H2O (2×75 mL) and brine (1×75 mL), then dried over Na2SO4, filtered and concentrated. The crude product is purified by chromatography using hexane to give the title compound (1.07 gm, 81% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07557103B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-f885c5b69ce64084a3526fa07ea4d8af |
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| 出典メモ | uspto-grants-2009_07 |
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