関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | 4-Bromodiphenyl Ether | HCID 7565 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Propanone, 2,2-dimethyl-1-(4-phenoxyphenyl)- | HCID 41633 | — |
反応手順
To a flask containing 33.6 g. of magnesium and a few crystals of iodine, is added 50 to 70 ml. of a solution of 300 g. of 4-bromodiphenyl ether in 500 ml. of absolute tetrahydrofuran. The remainder of the solution is added as needed to maintain a gentle reflux and the resulting mixture heated to reflux for 30 minutes. The resulting mixture is then added to a solution of trimethylacetyl chloride in 500 ml. of absolute tetrahydrofuran at a rate so as to maintain a temperature of from 40° to 50° C. The resulting mixture is then stirred at ambient temperature for 1 hour. 200 ml. of 2N. hydrochloric acid is then added. The organic layer is washed twice with 1 liter of 2N. sodium carbonate solution, dried and evaporated in vacuo to a liquid. The liquid thus obtained is distilled under reduced pressure to obtain p-phenoxypivalophenone, b.p. 136°-139° C. at 0.1 mm/Hg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03985883 |
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| 出典データセット | uspto-grants-1976_10 |
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| ORD ID | ord-ba6552a9c99b403d8ef1e3f22c702d3e |
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| 出典メモ | uspto-grants-1976_10 |
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