関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 1-Bromo-3,4,5-trifluorobenzene | HCID 611409 | — |
| 反応物 | 3',4',5'-Trifluoroacetophenone | HCID 2776907 | — |
| 生成物 | HCID 18783754 | HCID 18783754 | — |
反応手順
3,4,5-Trifluorophenol (5.0 g, 0.034 mol), which was obtained by reacting a Grignard reagent of 1-bromo-3,4,5-trifluorobenzene with acetyl chloride, oxidizing the resulting 1-acetyl-3,4,5-trifluorobenzene with a peracid to obtain 3,4,5-trifluorophenyl acetate and subjecting this acetate to hydrolysis reaction, was dissolved in dry pyridine (10 ml), followed by gradually adding trans-4-propyl-cyclohexylcarbonyl chloride (6.4 g), allowing the resulting reaction solution to stand at 50° C. for 3 hours, adding water (100 ml) to the reaction solution, extracting the resulting deposited oily substance with n-heptane (30 ml), washing the n-heptane solution with a dilute hydrochloric acid aqueous solution and then with a dilute alkali aqueous solution, further washing with water till the washing water became neutral, drying the n-heptane solution over anhydrous sodium sulfate, distilling off n-heptane and recrystallizing the resulting oily substance from ethyl alcohol to obtain 3,4,5-trifluorophenyltrans-4-propylcyclohexyl carboxylate (6.5 g).C-I: 4.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05032313 |
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| 出典データセット | uspto-grants-1991_07 |
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| ORD ID | ord-34e9b7e974fe465da715fe8020440d1e |
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| 出典メモ | uspto-grants-1991_07 |
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