関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Triisopropylsilyl trifluoromethanesulfonate | HCID 2724529 | — |
| 反応物 | 4-(2,4,5-Trifluorophenyl)cyclohexanone | HCID 57424362 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Triisopropyl{[4-(2,4,5-trifluorophenyl)cyclohex-1-en-1-yl]oxy}silane | HCID 67065786 | — |
反応手順
A three-neck flask (1 L) containing a stirred solution of 4-(2,4,5-trifluorophenyl)cyclohexanone (15.8 g) in dichloromethane (160 mL) under a nitrogen atmosphere was cooled to 0° C. and then treated with triethylamine (22 mL) followed by triisopropylsilyl trifluoromethanesulfonate (25.4 g) while maintaining the temperature below 5° C. The solution was stirred at 0° for 30 min and then allowed to rise to ambient temperature over a period of 0.5 h. It was then treated with saturated aqueous ammonium chloride solution. The organic layer was separated, dried over anhydrous magnesium sulfate and evaporated. The crude product was chromatographed (silica gel, 3% ether in hexane) to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07906649B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-d4f395ba346b46dc933b09a0407c3940 |
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| 出典メモ | uspto-grants-2011_03 |
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