반응 #3009

반응 방정식

dichloromethane

dichloromethane

perfluorooctanesulfonic acid potassium salt

triphenylsulfonium chloride

→

triphenylsulfonium perfluorooctanesulfonate

용매

water

반응 조건

후처리

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

실험 절차

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).

출처