Reacción #2027193

ord-31149e0d3d5c4dc7928557d770e8d47e

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturaunder reflux for 2 hours
  3. 3
    Temperaturathe whole mixture was heated
  4. 4
    Temperaturaunder reflux for a further 30 minutes
  5. 5
    TemperaturaAfter the mixture had been cooled
  6. 6
    Otroto precipitate crystals
  7. 7
    FiltraciónThese crystals were collected by filtration
  8. 8
    Otrorecrystallized from ethanol

Procedimiento

A mixture of 2.5 g of 2-(4-t-butoxycarbonylaminophenyl)-3-oxobutyronitrile, 20 ml of ethanol and 1.4 g of 2,2-diethoxyethylhydrazine was heated under reflux for 2 hours. 20 ml of 4N hydrogen chloride in dioxane were added, and then the whole mixture was heated under reflux for a further 30 minutes. After the mixture had been cooled, ethyl acetate was added to precipitate crystals. These crystals were collected by filtration and recrystallized from ethanol to give 1.4 g of the title compound as pale brown plates melting at 180°-190° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05698576uspto-grants-1997_12