関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetraethoxysilane | HCID 6517 | — |
| 反応物 | Bromopentafluorobenzene | HCID 9578 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Bis(pentafluorophenyl)diethoxysilane | HCID 11102434 | — |
反応手順
265.2 mL (1.95 mol, 525.353 g) bromopentafluorobenzene, 52.11 g (2.144 mol) magnesium powder and 216 mL (0.975 molt 203.025 g) tetraethoxysilane are mixed together at room temperature and diethylether is added dropwise to the vigorously stirred solution until an exothermic reaction is observed (˜240 mL). The solution is stirred for 30 minutes after which additional 90 mL of Et2O is carefully added. After stirring at 35° C. for 16 h the mixture is cooled to room temperature and diethylether evaporated. An excess of n-heptane (˜600 mL) is added to precipitate the magnesium salts. Solution is filtrated and evaporated to dryness. The residue is fractionally distilled under reduced pressure to yield di(pentafluorophenyl)diethoxysilane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06924384B2 |
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| 出典データセット | uspto-grants-2005_08 |
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| ORD ID | ord-b49099e9420944be910de1a7a6310513 |
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| 出典メモ | uspto-grants-2005_08 |
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