Reacción #3009

Ecuación de reacción

dichloromethane

dichloromethane

perfluorooctanesulfonic acid potassium salt

triphenylsulfonium chloride

→

triphenylsulfonium perfluorooctanesulfonate

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGthe mixture stirred at room temperature for 20 hours
2. 2
   Otrothe layers separated
3. 3
   LavadoThe organic layer was washed with water (5×125 ml) until the washings
4. 4
   OtroAfter drying
5. 5
   Otro(MgSO4 ), removal of the solvent in vacuo
6. 6
   Otrogave a viscous gum which
7. 7
   Otrowas further dried
8. 8
   Temperaturaby heating at 80°-90° C. for 84 hours under vacuum

Procedimiento

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).

Fuente