関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Fluoroacryloyl chloride | HCID 2783335 | — |
| 反応物 | 2-(3,4-Dimethylphenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol | HCID 14438707 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(3,4-Dimethylphenyl)-hexafluoro-2-propyl alpha-fluoroacrylate | HCID 13980933 | 51.4% |
反応手順
A solution of 27.3 g (0.1 mol) Of 2-(3,4-dimethylphenyl)-hexafluoro-2-propanol and 10.1 g (0.1 mol) of triethylamine in 50 ml of dry diethyl ether was added dropwise with stirring at a temperature of 20° C. to a solution of 20 g (0.184 mol) of α-fluoroacryloyl chloride (obtained according to Example 4) in 50 ml of dry diethyl ether in the course of 35 minutes. The reaction mixture was then stirred at a temperature of 20° C. for a further 3.5 hours. The resulting solid was filtered off. The filtrate was distilled under reduced pressure after addition of 0.01 g of hydroquinone monomethyl ether. 17.7 g (51 percent of theory) of 2-(3,4-dimethylphenyl)-hexafluoro-2-propyl α-fluoroacrylate having a boiling point of 72° to 73° C. (under 0.4 mbar) were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05198925 |
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| 出典データセット | uspto-grants-1993_03 |
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| ORD ID | ord-721cf85334564ec9b439150cfb1efb78 |
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| 出典メモ | uspto-grants-1993_03 |
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