関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-Chloro-2,4-difluoro-5-nitrobenzene | HCID 73867 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-Fluoro-4-(2,2,2-trifluoroethoxy)-5-chloronitrobenzene | HCID 19887653 | — |
反応手順
22.5 g of 88% potassium hydroxide are suspended in 120 ml of dimethyl sulfoxide. With stirring, 40 g of trifluoroethanol are added dropwise to this suspension. Then, also with stirring, the resultant solution is added dropwise at room temperature to a solution of 96.8 g of 2,4-difluoro-5-chloronitrobenzene in 150 ml of dimethyl sulfoxide. When the addition is complete, the reaction mixture is stirred for a further 2 hours at room temperature. The reaction mixture is then concentrated, the crude product is dissolved in methylene chloride, and the resultant solution is washed with water and dried. Finally, the solvent is distilled off. Purification is effected by chromatography through a column of silica gel with a 10:1 mixture of hexane and ether as eluant. The solvent is distilled off, affording the title compound of the formula ##STR10## in the form of yellow crystals; m.p.: 54°-55° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05132325 |
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| 出典データセット | uspto-grants-1992_07 |
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| ORD ID | ord-30de927fa5ff45019fd563ab1c6cd524 |
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| 出典メモ | uspto-grants-1992_07 |
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