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Dichloromethane → Triphenylsulfonium perfluorooctanesulfonate

HRID 2913
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2913
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Komponenten

5

Edukt 3

HCID 6344Dichloromethane2×HCID 61343Triphenylsulfonium chlorideHCID 23669238Potassium perfluorooctanesulfonate

Produkt 1

HCID 21863781Triphenylsulfonium perfluorooctanesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  1. stirringthe mixture stirred at room temperature for 20 hours
  2. customthe layers separated
  3. washThe organic layer was washed with water (5×125 ml) until the washings
  4. customAfter drying
  5. custom(MgSO4 ), removal of the solvent in vacuo
  6. customgave a viscous gum which
  7. customwas further dried
  8. temperatureby heating at 80°-90° C. for 84 hours under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-d1e6e90adf2744bfa6b435f6c7114ace
Quelldatensatz
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05731364

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