Реакция #502063

ord-5a8415d00d4646b4972e7d00f9d6914e

Уравнение реакции

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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ПромывкаThe chloroform layer was washed several times with water
  2. 2
    Сушкаdried over anhydrous sodium sulfate
  3. 3
    Фильтрацияfiltered
  4. 4
    Другоеthe 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
    ДругоеA white precipitate formed
  8. 8
    ФильтрацияThe mixture was filtered
  9. 9
    Другоеrecovered precipitate
  10. 10
    Другоеwas dried under vacuum
  11. 11
    Другоеresulting in a white powder

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08088548B2uspto-grants-2012_01