반응 #502063

ord-5a8415d00d4646b4972e7d00f9d6914e

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The chloroform layer was washed several times with water
  2. 2
    건조dried over anhydrous sodium sulfate
  3. 3
    여과filtered
  4. 4
    기타the 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
    기타A white precipitate formed
  8. 8
    여과The mixture was filtered
  9. 9
    기타recovered precipitate
  10. 10
    기타was dried under vacuum
  11. 11
    기타resulting in a white powder

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08088548B2uspto-grants-2012_01