関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Fluoroacryloyl chloride | HCID 2783335 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Trifluoromethylphenyl alpha-fluoroacrylate | HCID 14512541 | 68.2% |
反応手順
27.5 g (0.169 mol) of 3-trifluoromethylphenol were dissolved in 100 ml of anhydrous methylene dichloride, and 17.1 g (0.169 mol) of triethylamine were added in portions to the solution; 20 g (0.184 mol) of α-fluoroacryloyl chloride (obtained in accordance with example 1c) were then added dropwise, at a temperature of 5° C., with stirring and in the course of 20 minutes, and the reaction mixture was stirred for a further 60 minutes at the same temperature. The solid formed was filtered off and washed with 30 ml of methylene dichloride. The mixture of filtrate and wash solution was distilled, after adding 0.01 g of hydroquinone monomethyl ether. 27 g (68% of theory) of 3-trifluoromethylphenyl α-fluoroacrylate were obtained, boiling point 78° to 79° C. (under 4 mbar).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05266668 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-38e232f4472844959dfb9e3b4691fbbe |
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| 出典メモ | uspto-grants-1993_11 |
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