Reaktion #1246187

ord-d5e9690b5efa4d97bc82464d6124b039

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeby irradiating microwaves
  2. 2
    Sonstigeterminated
  3. 3
    Sonstigethe reaction
  4. 4
    Waschenwashed with water
  5. 5
    TrocknenThe organic layer was dried over anhydrous magnesium sulfate
  6. 6
    Einengenconcentrated
  7. 7
    Sonstigevacuum evaporation
  8. 8
    SonstigeThe residue was re-crystallized in dichloromethane

Vorschrift

2′,6′-Difluoroacetophenone (0.468 g, 3 mmol) was dissolved in anhydrous hydrazine (2 ml), followed by irradiating microwaves thereon with stirring at 150° C. for 5 min. The addition of water (0.5 ml) at 0° C. terminated the reaction. Afterwards, the reaction solution was diluted with ethyl acetate (10 ml) and washed with water. The organic layer was dried over anhydrous magnesium sulfate and concentrated using vacuum evaporation. The residue was re-crystallized in dichloromethane to give the title compound (Yield 85%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07812045B2uspto-grants-2010_10