関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4-Difluorophenol | HCID 123051 | — |
| 反応物 | 3-Bromo-4-fluorobenzotrifluoride | HCID 144295 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Bromo-1-(2,4-difluorophenoxy)-4-(trifluoromethyl)benzene | HCID 89656289 | 80.5% |
反応手順
A mixture of 3-bromo-4-fluorobenzotrifluoride (0.5 mL, 3.52 mmol), 2,4-difluorophenol (0.337 mL, 3.52 mmol), and potassium carbonate (0.486 g, 3.52 mmol) in dimethylformamide (7 mL) was heated at 80° C. overnight. The reaction mixture was cooled to ambient temperature and partitioned between ethyl acetate and water. The layers were separated, and the aqueous layer was extracted with ethyl acetate. The combined organics were washed with water and saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation. The crude material was purified by flash chromatography (ethyl acetate/hexanes) to provide the title compound (1.0 g, 80% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09050346B2 |
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| 出典データセット | uspto-grants-2015_06 |
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| ORD ID | ord-8058b1143cce49648c28259edfb111e8 |
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| 出典メモ | uspto-grants-2015_06 |
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