反応 #502063

ord-5a8415d00d4646b4972e7d00f9d6914e

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The chloroform layer was washed several times with water
  2. 2
    乾燥dried over anhydrous sodium sulfate
  3. 3
    ろ過filtered
  4. 4
    その他the 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
    その他A white precipitate formed
  8. 8
    ろ過The mixture was filtered
  9. 9
    その他recovered precipitate
  10. 10
    その他was dried under vacuum
  11. 11
    その他resulting in a white powder

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08088548B2uspto-grants-2012_01