Reacción #578431

ord-497033c00cf94772b16745e935eee3ec

Ecuación de reacción

[Cl-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium chloride
Cc1ccc(S(=O)(=O)OCC(F)(F)S(=O)(=O)[O-])cc1.[Na+]
sodium 1,1-difluoro-2-tosyloxyethanesulfonate
Cc1ccc(S(=O)(=O)OCC(F)(F)S(=O)(=O)[O-])cc1.c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium 1,1-difluoro-2-tosyloxyethanesulfonate
Rendimiento 74.0%

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrosynthesized in Synthesis Example 9
  2. 2
    OtroThe organic layer was separated
  3. 3
    Lavadowashed with 20 g of water three times
  4. 4
    ConcentraciónThe organic layer was concentrated
  5. 5
    workup.ADDITION10 g of diisopropyl ether was added to the residue for crystallization
  6. 6
    FiltraciónThe crystals were filtered
  7. 7
    Otrodried
  8. 8
    Otroobtaining the target compound

Procedimiento

To 62 g of dichloromethane were added an amount (corresponding to 0.031 mole) of the triphenylsulfonium chloride aqueous solution of Synthesis Example 1 and 1.1 g (0.033 mole) of sodium 1,1-difluoro-2-tosyloxyethanesulfonate synthesized in Synthesis Example 9, followed by stirring. The organic layer was separated and washed with 20 g of water three times. The organic layer was concentrated and 10 g of diisopropyl ether was added to the residue for crystallization. The crystals were filtered and dried, obtaining the target compound. White crystals, 1.3 g (yield 74%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07531290B2uspto-grants-2009_05