Reaktion #2501397

ord-b85de126c89e4f0ba17534802131e14e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling down
  2. 2
    Sonstigethe mixture vigorously stirred overnight
  3. 3
    FiltrationFiltration
  4. 4
    Waschenwashing with ethyl ether
  5. 5
    Sonstigeyielded a brown solid, which
  6. 6
    Filtrationthe solution filtered
  7. 7
    Sonstigethe water removed in vacuo
  8. 8
    Filtrationthe mixture filtered
  9. 9
    Waschenthe residue washed with ethyl ether

Vorschrift

Di-(2-thienyl)sulfide (2.1 g, 0.0104 mole), diphenyliodonium triflate (5.8 g, 0.0135 mole) and copper benzoate (0.08 g, 0.003 mole) are heated without solvent for 3 hours at 120-145° C. under a nitrogen atmosphere. After cooling down, 75 ml ethyl ether was added and the mixture vigorously stirred overnight to achieve solidification. Filtration and washing with ethyl ether yielded a brown solid, which was dissolved in hot water, the solution filtered and the water removed in vacuo. The resulting white solid was stirred in 50 ml ethyl ether for 24 hours, the mixture filtered and the residue washed with ethyl ether, yielding 3.4 g (78%) of the title compound, di(2-thienyl)phenylsulfonium triflate. The structure was confirmed by 1H/13C NMR spectroscopy.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06811961B2uspto-grants-2004_11