関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Triphenylsulfonium chloride | HCID 61343 | — |
| 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 (24.64 g, 46.1 mmol) in water (150 ml) at room temperature under nitrogen was added dropwise triphenylsulfonium chloride (50% aqueous solution, 27.50 g) over 15 minutes. After stirring the suspension for 30 minutes, dichloromethane (75 ml) was added and the mixture stirred at room temperature for 20 hours. Additional dichloromethane (225 ml) was added and the layers separated. The organic layer was washed with water (5×125 ml) until the washings were neutral (pH 7 ). After drying (MgSO4 ), removal of the solvent in vacuo gave a viscous gum which was further dried by heating at 80°-90° C. for 84 hours under vacuum. In this way, triphenylsulfonium perfluorooctanesulfonate was isolated as a glassy solid (30.61 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05731364 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-d1e6e90adf2744bfa6b435f6c7114ace |
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| 出典メモ | uspto-grants-1998_03 |
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