関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 2,3-Difluorophenol | HCID 80879 | — |
| 反応物 | Potassium | HCID 5462222 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2,3-Difluorobenzene-1,4-diol | HCID 11029970 | — |
反応手順
1 mol of 2,3-difluorophenol is dissolved in 1 l of 10% sodium hydroxide solution, and a saturated aqueous solution of 1.1 mol of potassium peroxodisulphate is added dropwise over the course of 4 hours with ice cooling. During this addition, the temperature must not exceed 20o The mixture is stirred overnight at room temperature and neutralized using hydrochloric acid, and unreacted starting material is extracted with ether. 3 1 of toluene and 2 mol of sodium sulphite are added to the aqueous phase, and the mixture is strongly acidified using 1 1 of concentrated hydrochloric acid and refluxed for 20 minutes. After cooling, the toluene layer is separated off, the aqueous phase is extracted with ether in a perforator, and 2,3-difluorohydroquinone is obtained by evaporating the combined toluene and ether extracts.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05248447 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-32048f4b38654a34b265cba539771b47 |
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| 出典メモ | uspto-grants-1993_09 |
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