Réaction #502063

ord-5a8415d00d4646b4972e7d00f9d6914e

Équation de réaction

O=S(=O)([O-])C(F)(F)C(F)(F)C(F)(F)C(F)(F)S(=O)(=O)[O-].[K+].[K+]
Perfluorobutane-1,4-disulfonic acid potassium salt
[Br-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium bromide
ClC(Cl)Cl
Chloroform
O=S(=O)([O-])C(F)(F)C(F)(F)C(F)(F)C(F)(F)S(=O)(=O)[O-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1.c1ccc([S+](c2ccccc2)c2ccccc2)cc1
bis(triphenylsulfonium) perfluorobutane-1,4-disulfonate

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    LavageThe chloroform layer was washed several times with water
  2. 2
    Séchagedried over anhydrous sodium sulfate
  3. 3
    Filtrationfiltered
  4. 4
    Autrethe filtrate evaporated to an oil stage
  5. 5
    workup.ADDITIONEther was added to the oil
  6. 6
    workup.STIRRINGthe mixture was stirred vigorously
  7. 7
    AutreA white precipitate formed
  8. 8
    FiltrationThe mixture was filtered
  9. 9
    Autrerecovered precipitate
  10. 10
    Autrewas dried under vacuum
  11. 11
    Autreresulting in a white powder

Mode opératoire

Perfluorobutane-1,4-disulfonic acid potassium salt (2.5 g) was added to a solution of triphenylsulfonium bromide (3.5 g) in 150 ml of water. Chloroform (150 ml) was added and stirred for 5 hours. The chloroform layer was washed several times with water, dried over anhydrous sodium sulfate, filtered, and the filtrate evaporated to an oil stage. Ether was added to the oil and the mixture was stirred vigorously. A white precipitate formed. The mixture was filtered and recovered precipitate was dried under vacuum, resulting in a white powder; mp 155° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08088548B2uspto-grants-2012_01