反应 #502063

ord-5a8415d00d4646b4972e7d00f9d6914e

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤The chloroform layer was washed several times with water
  2. 2
    干燥dried over anhydrous sodium sulfate
  3. 3
    过滤filtered
  4. 4
    其他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
    其他A white precipitate formed
  8. 8
    过滤The mixture was filtered
  9. 9
    其他recovered precipitate
  10. 10
    其他was dried under vacuum
  11. 11
    其他resulting in a white powder

实验过程

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.

来源

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