Реакция #2195486

ord-26e51e4bbb7542dfa6828d6528aeb819

Уравнение реакции

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
Выход 43.0%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеat 85° C.
  2. 2
    Другоеfor 65 hours
  3. 3
    Температураto cool
  4. 4
    Другоеto separate a water layer
  5. 5
    workup.ADDITIONA saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals
  6. 6
    ФильтрацияThe crystals were collected by filtration
  7. 7
    Промывкаwashed with a small volume of saturated sodium chloride aqueous solution
  8. 8
    Другоеdried in vacuum

Методика

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. The reaction took place at 85° C. for 65 hours. The reaction solution was allowed to cool. 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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07514202B2uspto-grants-2009_04