関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (1,1'-Biphenyl)-2-ol | HCID 7017 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Bromo-2-fluorobenzonitrile | HCID 2724900 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(Biphenyl-2-yloxy)-5-bromo-benzonitrile | HCID 59436590 | 89% |
反応手順
A suspension of 5-bromo-2-fluorobenzonitrile (6.48 g, 32.4 mmol), 2-phenylphenol (5.79 g, 34 mmol) and potassium carbonate (4.92 g, 35.6 mmol) in DMF (50 ml) was heated at 70° C. for 3 hours. The reaction was cooled and quenched by the addition of water (200 ml) followed by extraction with tBuOMe. The organic layer was dried (MgSO4) and concentrated in vacuo. The residue was purified using silica gel column chromatography (ethyl acetate:Heptane 5:95 to 15:85) to furnish 10.1 g of the desired compound. LCMS Rt=1.78 min MS m/z 349 [M]+1HNMR (d6-DMSO): δ 6.6 (m, 1H), 7.2-7.6 (m, 9H), 7.65 (m, 1H), 8.0 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541588B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-c2524a5135f547338c10b1fc44b5fda2 |
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| 出典メモ | uspto-grants-2013_09 |
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