Reaktion #2161239

ord-e10bcd3a857e41448b4796a72dc2cde4

Reaktionsgleichung

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

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeprepared in Synthesis Example 14
  2. 2
    Temperaturwas heated
  3. 3
    WaschenThe organic layer was washed with 30 g of water three times
  4. 4
    Einengenconcentrated
  5. 5
    workup.ADDITIONDiethyl ether was added to the
  6. 6
    Einengenconcentrate for crystallization
  7. 7
    FiltrationThe crystals were filtered
  8. 8
    Sonstigedried
  9. 9
    Sonstigeobtaining the target compound in an amount of 4.9 g

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07919226B2uspto-grants-2011_04