Reaktion #7319

ord-8b47c9918eef431b95489edd655f8465

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturreflux
  2. 2
    Temperaturcooling
  3. 3
    workup.STIRRINGThe solution is stirred for one hour at a temperature of 60° C. and subsequently for a further 3 hours at 110° C
  4. 4
    workup.DISTILLATIONAfter distillation, 5.41 g of methyl pentafluoroethanesulfonate
  5. 5
    Sonstigeare isolated (boiling range: 114–115° C., yield: 84.1%)

Vorschrift

5.74 g (15.0 mmol) of pentafluoroethanesulfonic anhydride and 0.31 g (1.55 mmol) of pentafluoroethanesulfonic acid are initially introduced in a 10 ml round-necked flask. 1.35 g (15.0 mmol) of dimethyl carbonate are added at room temperature with constant stirring and reflux cooling. The solution is stirred for one hour at a temperature of 60° C. and subsequently for a further 3 hours at 110° C. After distillation, 5.41 g of methyl pentafluoroethanesulfonate are isolated (boiling range: 114–115° C., yield: 84.1%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07084290B2uspto-grants-2006_08