Reacción #62532

ord-6556d3199ab54b82bec6064b8264157e

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturarefluxed
  2. 2
    Temperaturaunder heating for 6 hours
  3. 3
    FiltraciónThe reaction mixture was filtered in hot state
  4. 4
    Temperaturathe filtrate was cooled
  5. 5
    Filtraciónwas collected by filtration

Procedimiento

2,4-dinitroaniline (18.05 g), triethylamine (12.97 g) and benzene (750 ml) were placed in a reaction vessel and stirred under the nitrogen atmosphere. To the reaction mixture, 3,5-dinitrobenzoyl chloride (25.00 g) was added and refluxed under heating for 6 hours. The reaction mixture was filtered in hot state and the filtrate was cooled to deposit crystals of 2',3,4',5-tetranitrobenzanilide which was collected by filtration. The product of 2',3,4',5-tetranitrobenzanilide (3.00 g) thus obtained, platinum/carbon (5%) (0.18 g) and dioxane (85 ml) were placed in a pressurized vessel and allowed to react under the hydrogen pressure of 1 to 3 kg/cm2 at 80° C. for 10 hours. After cooling, the catalyst was removed by filtration and dioxane was distilled off under the reduced pressure to obtain powder of 2',3,4',5-tetraaminobenzanilide.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04761234uspto-grants-1988_08