関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon tetrafluoride | HCID 6393 | — |
| 反応物 | 1,1,1,4,5,5,5-Heptafluoro-3-(pentafluoroethyl)-2,4-bis(trifluoromethyl)pent-2-ene | HCID 121670 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | (Trifluoromethyl)trimethylsilane | HCID 552549 | — |
| 反応物 | 1,1,1,5,5,5-Hexafluoro-3-[1-(trifluoromethyl)-1,2,2,2-tetrafluoroethyl]-2,4,4-tris(trifluoromethyl)-2-pentene | HCID 22642015 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Perfluoro 4,4-dimethyl-3-isopropyl-2-pentene | HCID 73990785 | — |
反応手順
1 mmol (450 mg) of perfluoro(3-ethyl-2,4-dimethyl-2-pentene) and 4.0 mmol (568.8 mg) of trifluoromethyltrimethylsilane were weighed into a 10-ml fluororesin-made reaction container, then 1 ml of dimethyl formamide and 0.1 mmol of acidic potassium fluoride (KHF2, 7.8 mg) were added therein. A fluororesin-made magnetic stirrer was placed and the mixture was stirred vigorously for 1 hour at room temperature, and then 1.0 mmol of trifluoromethyltrimethylsilane (142.2 mg) and 0.1 mmol of acidic potassium fluoride (KHF2, 7.8 mg) were added and the mixture was further stirred vigorously for 1 hour at room temperature. After completion of the reaction, the transparent lower perfluorocarbon layer was analyzed by gas chromatography using a capillary column (NB-1, 0.25 μm, 1.5 mm ID×60 m). The yield of the main product perfluoro(2,4,4-trimethyl-3-isopropyl-2-pentene) was 74.5% by weight. As the by-product, perfluoro 4,4-dimethyl-3-isopropyl-2-pentene was obtained at the yield of 25.5% by weight. The starting material perfluoro(3-ethyl-2,4-dimethyl-2-pentene) was consumed completely by the reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06710214B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-13ce255a86bf4c28b9543ff9474bc153 |
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| 出典メモ | uspto-grants-2004_03 |
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