Réaction #2161239

ord-e10bcd3a857e41448b4796a72dc2cde4

Équation de réaction

CC(C)(C)Oc1ccc([S+](c2ccccc2)c2ccccc2)cc1.O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1
4-tert-butoxyphenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate
CS(=O)(=O)O
Methanesulfonic acid
O=C(OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-])c1ccccc1.Oc1ccc([S+](c2ccccc2)c2ccccc2)cc1
(4-hydroxyphenyl)diphenylsulfonium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate

Conditions de réaction

Température
40°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autreprepared in Synthesis Example 14
  2. 2
    Températurewas heated
  3. 3
    LavageThe organic layer was washed with 30 g of water three times
  4. 4
    Concentrationconcentrated
  5. 5
    workup.ADDITIONDiethyl ether was added to the
  6. 6
    Concentrationconcentrate for crystallization
  7. 7
    FiltrationThe crystals were filtered
  8. 8
    Autredried
  9. 9
    Autreobtaining the target compound in an amount of 4.9 g

Mode opératoire

In 60 g of dichloromethane was dissolved 6.7 g of 4-tert-butoxyphenyldiphenylsulfonium 1,1,3,3,3-pentafluoro-2-benzoyloxypropane-1-sulfonate (PAG4) prepared in Synthesis Example 14. Methanesulfonic acid, 0.1 g, was added to the solution, which was heated and stirred at 40° C. for 3 hours. The organic layer was washed with 30 g of water three times, and concentrated. Diethyl ether was added to the concentrate for crystallization. The crystals were filtered and dried, obtaining the target compound in an amount of 4.9 g.

Source

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