Reacción #4478

ord-78fc489b6c4b4be39c7bb6d9b5564ba7

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated
  2. 2
    Temperaturato reflux for 14 h
  3. 3
    Temperaturato cool
  4. 4
    Filtraciónthe precipitate filtered
  5. 5
    Lavadowashed with isopropyl acetate and ether
  6. 6
    Otroto give a solid
  7. 7
    OtroRecrystallisation from methanol

Procedimiento

1,3-Cyclohexanedione (3.1 g) and the product of Stage (i) (5.6 g) in ethanol (196 ml) and water (39 ml) was stirred at room temperature for 3 h and then heated to reflux for 14 h. The resulting solution was allowed to cool, poured into water (500 ml) and the precipitate filtered and washed with isopropyl acetate and ether to give a solid. Recrystallisation from methanol gave the title compound as a solid (2.5 g) m.p. 235°-237°.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04725615uspto-grants-1988_02