Reacción #53247

ord-71bd1248fad64cd58c8f6ed57ff96111

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroa solution obtained
  2. 2
    workup.ADDITIONwas added to the above solution
  3. 3
    ExtracciónThe aqueous solution was extracted twice with 100 ml of chloroform
  4. 4
    Lavadothe organic phase was washed with water
  5. 5
    Concentraciónconcentrated
  6. 6
    Otroan oily product was obtained
  7. 7
    ConcentraciónThe above-obtained product was concentrated again with ethyl acetate
  8. 8
    Otroa solid product was obtained
  9. 9
    FiltraciónThe solid product was filtered and re-slurried with diisopropyl ether

Procedimiento

Potassium perfluorobutanesulfonate (10 g) was dissolved in a mixed solvent comprising 500 ml of water and 100 ml of methanol, and a solution obtained by dissolving 7.7 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide in 50 ml of methanol was added to the above solution. The aqueous solution was extracted twice with 100 ml of chloroform, the organic phase was washed with water and concentrated, thereby an oily product was obtained. The above-obtained product was concentrated again with ethyl acetate, thereby a solid product was obtained. The solid product was filtered and re-slurried with diisopropyl ether, to thereby obtain 9 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06858370B2uspto-grants-2005_02