関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromo-2-fluorophenol | HCID 2724981 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 3-Fluoro-4-hydroxybenzonitrile | HCID 2782944 | 96.2% |
反応手順
4-Bromo-2-fluorophenol (10 ml, 91 mmol) and 9.85 g (0.11 mol) of CuCN were combined in 75 ml of NMP with stirring under nitrogen, and the mixture was heated at 150° C. for 5 h. The mixture was diluted with 200 ml of ether, stirred, and decanted. The residue was diluted again with 200 ml of ether, heated, and decanted. The combined decantates were washed with water, 1N HCl solution, water, and brine, and dried over magnesium sulfate. The organic solution was concentrated in vacuo to provide 12 g of a white solid which was triturated in carbon tetrachloride and filtered to afford 7.29 g (72.1%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05643929 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-a9f37634b6b8400d9b8a6ba72ce3732a |
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| 出典メモ | uspto-grants-1997_07 |
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