Reaktion #6907

ord-ce024ddd171d42738801fd911c4752bb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe tube was flushed with nitrogen
  2. 2
    Sonstigesealed
  3. 3
    TemperaturThe sealed tube was heated at 100° for 3.5 h
  4. 4
    Filtrationthe resulting solids filtered
  5. 5
    Waschenwashed with acetonitrile
  6. 6
    workup.DISSOLUTIONThe solids were dissolved in chloroform
  7. 7
    Sonstigethe solvent removed under vacuum
  8. 8
    Sonstigeto provide a solid

Vorschrift

In a heavy-walled PYREX tube was placed 2-iodoaniline (2.84 g, 13 mmol), dimethylmaleate (2.44 g, 17 mmol), triethylamine (1.4 mL, 10 mmol), palladium diacetate (31 mg, 0.14 mmol) and 6 mL acetonitrile. The tube was flushed with nitrogen and sealed. The sealed tube was heated at 100° for 3.5 h then cooled to r.t. The tube was opened and the resulting solids filtered and washed with acetonitrile. The solids were dissolved in chloroform and the solvent removed under vacuum to provide a solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07084156B2uspto-grants-2006_08