Reacción #1463489

ord-4b619910aa744d42828a8ffc7b87d55a

Disolventes

Condiciones de reacción

Temperatura
180°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe reaction vessel was sealed
  2. 2
    Temperaturamaintained at that temperature for 12 hours
  3. 3
    OtroThe oil bath was removed
  4. 4
    ExtracciónThe solid was extracted with methylene chloride
  5. 5
    Otrothe insoluble materials removed by filtration
  6. 6
    OtroThe solvent was removed
  7. 7
    Otrothe solid recrystallized from hot methanol
  8. 8
    OtroThe material was chromatographed on a silica gel column

Procedimiento

A Parr stainless steel high pressure reactor was charged with 1-chloroanthraquinone (24.3 g), 1-ethylpropylamine (17.5 g), potassium acetate.(14.0 g), activated copper metal (0.7 g), and water (0.05 g). The reaction vessel was sealed and heated to a temperature of 180° C. in an oil bath and maintained at that temperature for 12 hours. The oil bath was removed and the vessel was allowed to return to ambient conditions. The solid was extracted with methylene chloride and the insoluble materials removed by filtration. The solvent was removed and the solid recrystallized from hot methanol. The material was chromatographed on a silica gel column using toluene as the eluent.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05663024uspto-grants-1997_09