반응 #7319

ord-8b47c9918eef431b95489edd655f8465

반응 방정식

O=S(=O)(OS(=O)(=O)C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)F
pentafluoroethanesulfonic anhydride
O=S(=O)(O)C(F)(F)C(F)(F)F
pentafluoroethanesulfonic acid
COC(=O)OC
dimethyl carbonate
COS(=O)(=O)C(F)(F)C(F)(F)F
methyl pentafluoroethanesulfonate
수율 84.1%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도reflux
  2. 2
    온도cooling
  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
    기타are isolated (boiling range: 114–115° C., yield: 84.1%)

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084290B2uspto-grants-2006_08