関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Triphenylsulfonium Bromide | HCID 11984010 | — |
| 反応物 | Potassium perfluorooctanesulfonate | HCID 23669238 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Triphenylsulfonium perfluorooctanesulfonate | HCID 21863781 | — |
反応手順
To a suspension of perfluorooctanesulfonic acid potassium salt (10.76 g, 20.0 mmol) in water (100 mL) at room temperature under nitrogen was added dropwise triphenylsulfonium bromide (6.87 g, 20.0 mmol) over 15 min. After stirring the suspension for 30 min., dichloromethane (100 mL) was added and the biphasic mixture stirred at room temperature for 20 h. Additional dichloromethane (100 mL) was added and the layers separated. The organic layer was washed with water (3×75 mL) until the washings were neutral (pH 7). After drying (MgSO4), removal of the solvent in vacuum gave a viscous gum which was further dried by heating at 50° C. for 24 h under vacuum. In this way, triphenylsulfonium perfluorooctanesulfonate was isolated as a pale yellow gummy solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06645698B1 |
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| 出典データセット | uspto-grants-2003_11 |
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| ORD ID | ord-33260386189244328ed78539ca8fe351 |
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| 出典メモ | uspto-grants-2003_11 |
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