Reacción #476181

ord-71609c6bf8684a39917da1e4d7f8d101

Ecuación de reacción

[Cl-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium chloride
O=C([O-])C(F)(F)S(=O)(=O)O.[Na+]
sodium difluorosulfoacetate
O=C(O)C(F)(F)S(=O)(=O)[O-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium hydroxycarbonyldifluoromethanesulfonate

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe mixture was filtered
  2. 2
    Otroto obtain white solid and white solid
  3. 3
    Otroobtained
  4. 4
    Lavadowas washed with 150 parts of ion-exchanged water
  5. 5
    workup.ADDITION506 Parts of tert-butyl methyl ether was added to white solid
  6. 6
    Otroobtained
  7. 7
    Filtraciónfiltered
  8. 8
    Otroto obtain solid
  9. 9
    OtroThe solid obtained
  10. 10
    Otrowas dried

Procedimiento

Into 2036 parts of 11.2% aqueous triphenylsulfonium chloride solution, 859 parts of 17.6% aqueous sodium difluorosulfoacetate solution was added and the resultant mixture was stirred at 25° C. for about 20 hours. The mixture was filtered to obtain white solid and white solid obtained was washed with 150 parts of ion-exchanged water. 506 Parts of tert-butyl methyl ether was added to white solid obtained. The resultant mixture was stirred and filtered to obtain solid. The solid obtained was dried to obtain 246.9 parts of triphenylsulfonium hydroxycarbonyldifluoromethanesulfonate, which is called as TPS-1.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08378016B2uspto-grants-2013_02