Réaction #2161237

ord-9103bfa7028849b1a9c2e5d4579bdca4

Équation de réaction

Cc1ccccc1
toluene
O=C(OC(=C(F)F)C(F)(F)F)c1ccccc1
1,1,3,3,3-pentafluoropropen-2-yl benzoate
O=S([O-])O.[Na+]
sodium hydrogen sulfite
O=C(OOC(=O)c1ccccc1)c1ccccc1
benzoyl peroxide
O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1.[Na+]
sodium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate
Rendement 43.0%

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreReaction
  2. 2
    Températureto cool
  3. 3
    Autreto separate a water layer
  4. 4
    workup.ADDITIONA saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals
  5. 5
    FiltrationThe crystals were collected by filtration
  6. 6
    Lavagewashed with a small volume of saturated sodium chloride aqueous solution
  7. 7
    Autredried in vacuum

Mode opératoire

10.0 g of 1,1,3,3,3-pentafluoropropen-2-yl benzoate which had been synthesized by a conventional technique, was dispersed in 72 g of water, after which 12.0 g of sodium hydrogen sulfite and 1.24 g of benzoyl peroxide were added. Reaction occurred at 85° C. for 65 hours. The reaction solution was allowed to cool, after which toluene was added, followed by separatory operation to separate a water layer. A saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals settled out. The crystals were collected by filtration, washed with a small volume of saturated sodium chloride aqueous solution and then dried in vacuum, obtaining the target compound, sodium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate. White crystals, 5.85 g (yield 43%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07919226B2uspto-grants-2011_04