Reacción #1246187

ord-d5e9690b5efa4d97bc82464d6124b039

Disolventes

Condiciones de reacción

Temperatura
150°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroby irradiating microwaves
  2. 2
    Otroterminated
  3. 3
    Otrothe reaction
  4. 4
    Lavadowashed with water
  5. 5
    SecadoThe organic layer was dried over anhydrous magnesium sulfate
  6. 6
    Concentraciónconcentrated
  7. 7
    Otrovacuum evaporation
  8. 8
    OtroThe residue was re-crystallized in dichloromethane

Procedimiento

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%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07812045B2uspto-grants-2010_10