関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | [4-(4-Bromophenyl)phenyl]methanol | HCID 1393673 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Bromo-4'-methoxymethylbiphenyl | HCID 68193260 | 95% |
反応手順
(4′-Bromobiphenyl-4-yl)methanol (1.2 g, 4.6 mmol) was dissolved in tetrahydrofuran (20 mL), and methyl iodide (0.97 g, 6.8 mmol), and then sodium hydride (63%, 0.26 g, 6.8 mmol) were added under a nitrogen atmosphere at 4° C., followed by stirring at room temperature for 30 minutes. A saturated aqueous ammonium chloride solution was added to the reaction solution, followed by extraction with ethyl acetate. After the solvent was distilled off under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/dichloromethane), and a fraction corresponding to the Rf value=0.50 (hexane/dichloromethane=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (1.2 g, 4.3 mmol) as a white solid (yield 95%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08785462B2 |
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| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-5073859ddfc64a1e9600d1629e571b80 |
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| 出典メモ | uspto-grants-2014_07 |
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