関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Difluorophenol | HCID 80879 | — |
| 反応物 | 4-Chlorophenylacetyl chloride | HCID 90692 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(4-Chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-ethanone | HCID 68698513 | — |
反応手順
A mixture of aluminium chloride (7.66 g, 57.4 mmol, 1.5 eq.) and (4-chlorophenyl)acetyl chloride (8.7 g, 46 mmol, 1.2 eq.) in 1,2-dichloroethane (75 ml) is stirred at 0° C. for 30 min. A solution of 2,3-difluorophenol (5 g, 38.4 mmol) in 1,2-dichloroethane (25 ml) is added to the reaction mixture, which is heated in an oil bath at 90° C. overnight. The reaction mixture is cooled to room temperature, diluted with water and extracted with ethyl acetate. The organic phase is dried over anhydrous magnesium sulfate, filtered and evaporated to dryness in vacuo to afford a brown solid. This is triturated with hexane/ethyl acetate (9:1), filtered and dried to afford the title compound as a pale brown fine solid which is 87% pure by HPLC analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732435B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-9bbf5b40766140ed82fefb6b7021adb9 |
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| 出典メモ | uspto-grants-2010_06 |
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