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 | 59% |
反応手順
Anhydrous sodium acetate (139.3 mmol, 11.4 g) was added to a solution of the title compound of Example 14, Step A (3.24 mmol, 1.6 g) in acetic anhydride (70 mL) and heated for 3 hours at 110° C. After cooling, the reaction mixture was poured into water (100 mL) and stirred for 1 hour. The aqueous solution was extracted with ether (2×100 mL), washed with 3% aqueous KOH (2×20 mL) and water (2×20 mL). The washed ether layer was collected, dried, filtered and the filtrate was evaporated to a brown residue, which was purified by silica gel chromatography (eluent:hexanes) to obtain the desired product, 5-fluoro-3-methyl benzofuran (59%, 1.77 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06849629B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-7bd01e2abf8d4b599991aaf826873f13 |
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| 出典メモ | uspto-grants-2005_02 |
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