関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | 4-Bromodiphenyl Ether | HCID 7565 | — |
| 反応物 | 3-Acetylpyridine | HCID 9589 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | alpha-Methyl-alpha-(4-phenoxyphenyl)-3-pyridinemethanol | HCID 22768039 | — |
反応手順
25 ml. of a solution of 25.0 g. 4-bromodiphenylether in 75 ml. tetrahydrofuran is added to 2.5 g. magnesium and, admixed with a small crystal of iodine to initiate the Grignard reaction. Thereafter, the remainder of the solution is added dropwise to maintain gentle reflux. The Grignard solution is then refluxed for 0.5 hours, cooled to 5°-10° and to it is added dropwise 12.1 g. of 3-acetylpyridine. The reaction mixture is then stirred at room temperature for 16 hours, decomposed with saturated aqueous ammonium chloride solution and extracted with ether. The ether extracts are combined and after drying over anhydrous sodium sulfate, filtered and evaporated i.v. to dryness. From the residue is crystallized from pentane/ether, 1-(p-phenoxyphenyl)-1-(3-pyridyl)-ethan-1-ol, m.p. 130°-132°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04098908 |
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| 出典データセット | uspto-grants-1978_07 |
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| ORD ID | ord-9039b3d8daf742aaa5828c968021967a |
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| 出典メモ | uspto-grants-1978_07 |
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