Reacción #95398

ord-1bc5ffdd6ad2418a94a352058c4ea0a0

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas refluxed for one hour
  2. 2
    workup.DISTILLATIONThe solvent was then distilled off
  3. 3
    ExtracciónAfter extraction with ethyl acetate the aqueous phase
  4. 4
    workup.ADDITIONby addition of NaOH, whereby basic components
  5. 5
    Otroprecipitated in oily form
  6. 6
    Lavadothe organic phase was washed with water
  7. 7
    Secadodried over MgSO4
  8. 8
    Otroevaporated
  9. 9
    Otrothe solid residue was recrystallized twice from acetonitrile

Procedimiento

7.8 gm (0.03 mol) of 1-[2-cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane were dissolved in 80 ml of ethanol, and after addition of 7.5 gm (0.06 mol) of 1-ethinyl-cyclohexyl-amine the mixture was refluxed for one hour. The solvent was then distilled off, and the residue was acidified with dilute HCl. After extraction with ethyl acetate the aqueous phase was made alkaline by addition of NaOH, whereby basic components precipitated in oily form. They were taken up in ethyl acetate, the organic phase was washed with water, dried over MgSO4, evaporated and the solid residue was recrystallized twice from acetonitrile.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04344964uspto-grants-1982_08