関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Bromo-4-iodobenzene | HCID 11522 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | (Pentafluoroethyl)trimethylsilane | HCID 2760820 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Bromo-4-(pentafluoroethyl)benzene | HCID 54209708 | — |
反応手順
Under argon in a microwave vial 2 g 1-bromo-4-iodobenzene, 3.3 g trimethyl(perfluoroethyl)silane, 493 mg potassium fluoride and 2 g copper iodide are suspended in 10 ml N,N-dimethylformamide. The mixture is heated for 12 hours at 80° C. Further 3.3 g trimethyl(perfluoroethyl)silane are added and heating is continued for 48 hours. Then the mixture is partitioned between 2 M ammonia and diethylether. The aqueous phase is twice extracted with diethylether. The combined organic phases are washed three times with water and dried with magnesium sulphate. The solvent is evaporated in vacuo (300 mbar, temperature of water bath 50° C.). The residue is chromatographed on silica gel (dichloromethane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09029544B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-46f52acc79b14cd694f7e805bd7512fc |
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| 出典メモ | uspto-grants-2015_05 |
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