Reacción #83182

ord-2ab817c46ab84773bbd4994ae55649d7

Condiciones de reacción

Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrowas consumed
  2. 2
    workup.ADDITIONThe reaction was poured into water
  3. 3
    Extracciónextracted with ethyl acetate
  4. 4
    LavadoAfter washing with brine
  5. 5
    Secadothe organic phase was dried over magnesium sulfate
  6. 6
    Concentraciónconcentrated under vacuum
  7. 7
    Temperaturawithout heating
  8. 8
    OtroRemoval of the solvent
  9. 9
    Otrogave a foamy glassy solid which
  10. 10
    Otrowas triturated with hexane
  11. 11
    Filtraciónfiltered

Procedimiento

To a 500 mL flask was charged 100.0 g (0.38 mole) of alpha-(4-chlorophenyl)-alpha-ethyl-1H-1,2,4-triazole-1-propanenitrile and 100 mL of dimethyl sulfoxide. To the stirring solution was added 100 g (1.25 mole) of 50% sodium hydroxide. The reaction mixture was heated at 100° C. for 1 hour after which GLC indicated the starting material was consumed. The reaction was poured into water and extracted with ethyl acetate. After washing with brine, the organic phase was dried over magnesium sulfate and concentrated under vacuum without heating. Removal of the solvent gave a foamy glassy solid which was triturated with hexane, filtered and gave 97 g (91% yield) of a white solid, melting point 139°-140° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05624916uspto-grants-1997_04