関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Bromo-4-fluorophenylacetic Acid | HCID 3416339 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(3-Cyano-4-fluorophenyl)acetic acid | HCID 2773935 | 65% |
反応手順
To a solution of (3-bromo-4-fluoro-phenyl)-acetic acid (10 g, 42.9 mmol) in DMF (65 mL) was added copper (I) cyanide (7.7 g, 85.8 mmol) and heated at 130° C. for 24 hrs. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (250 mL). The organic layer was washed with water (5×50 mL), brine (50 mL), dried over sodium filtered and concentrated under reduced pressure. The crude material was re-crystallized from diethyl ether and hexane to afford the title compound as a yellow solid in 65% yield, 5 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846698B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-71110d3367f44455ae029b040795aa29 |
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| 出典メモ | uspto-grants-2014_09 |
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