関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Perfluorooctyl iodide | HCID 10491 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Phenylthiophenol | HCID 2760413 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Perfluorooctylthio)biphenyl | HCID 15655349 | 64% |
反応手順
To a solution composed of 40 ml of DMF and 4.66 g (25 mmol) of 2-mercaptobiphenyl was added 1.00 g (25 mmol) of sodium hydride (60% in oil) little by little under ice cooling and stirring. Then, 13.6 g (25 mmol) of perfluorooctyl iodide was added. The temperature of the mixture was slowly elevated to room temperature, and the mixture was stirred for 2 hours. Water was addd to the reaction mixture, and the mixture was extracted with hexane. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure to give a brown oil. It was purified by silica gel column chromatography using hexane as an eluent to give 9.60 g (64%) of 2-(perfluorooctylthio)biphenyl as a colorless oil. The properties of the product were as shown below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05066795 |
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| 出典データセット | uspto-grants-1991_11 |
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| ORD ID | ord-908ce0ba12bd4fb2ae01060942bb19b7 |
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| 出典メモ | uspto-grants-1991_11 |
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