تفاعل #977757
ord-189c2bb10ac24f4eb6b1b87233954f89
معادلة التفاعل
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المعالجة
- 1workup.STIRRINGthe biphasic mixture stirred at room temperature for 20 h
- 2أخرىthe layers separated
- 3غسيلThe organic layer was washed with water (3×75 mL) until the washings
- 4أخرىAfter drying
- 5أخرى(MgSO4), removal of the solvent in vacuum
- 6أخرىgave a viscous gum which
- 7أخرىwas further dried
الإجراء التجريبي
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.