関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-Iodobenzoyl chloride | HCID 74373 | — |
| 反応物 | 3-Buten-2-one, 4-methoxy- | HCID 94297 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(4-Iodo-phenyl)-5-methoxy-pent-4-ene-1,3-dione | HCID 67318321 | — |
反応手順
In a 1 ltr flask is cooled a solution of lithium hexamethyldisilazide (50 ml, 1.5 M) in THF (250 ml) to −75° C. During a period of 1 h is added 4-methoxy-but-3-en-2-one (6 ml). The mixture is stirred for 1 h at −70° C. A solution of 4-iodobenzoylchloride (7.2 g) in THF (250 ml) is added to the above mixture during 1 h at −70° C. The resulting mixture is slowly heated to ambient temperature and stirred for 1 h. Subsequently, the mixture is added to a cold aqueous solution of ammonium chloride and the resulting suspension is extracted with ethyl acetate. The organic phase is extracted twice with an aqueous solution of ammonium chloride, dried over sodium sulfate and evaporated. The crude oily product is transferred to the next step without any further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745446B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-da88ff71f72f4a34b33a1f2096cda387 |
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| 出典メモ | uspto-grants-2010_06 |
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