Reacción #170697

Ecuación de reacción

1-phenyl-5-(3-propylphenyl)-4,5-dihydro-1H-pyrazol-3-ylamine

→

titled compound

Rendimiento 47.0%

1-Phenyl-5-(3-propylphenyl)-1H-pyrazol-3-ylamine

Rendimiento 47.0%

Disolventes

toluene

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturaat reflux
2. 2
   Filtraciónthe activated carbon was filtered off through Celite
3. 3
   Lavadoeluted with ethyl acetate
4. 4
   ConcentraciónThis filtrate was concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONthe resulting residue was dissolved in toluene (185 ml)
6. 6
   workup.ADDITIONto the solution was added fresh activated carbon (pH5 to 8, 9.29 g)
7. 7
   workup.STIRRINGthe mixture was stirred overnight under oxygen atmosphere
8. 8
   Temperaturaat reflux
9. 9
   TemperaturaThis reaction solution was cooled to room temperature
10. 10
    Filtraciónthe activated carbon was filtered off through Celite
11. 11
    Lavadoeluted with ethyl acetate
12. 12
    ConcentraciónThis filtrate was concentrated under reduced pressure
13. 13
    Otrothe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=4/1 to 1/1)

Procedimiento

To a solution of the crude product of 1-phenyl-5-(3-propylphenyl)-4,5-dihydro-1H-pyrazol-3-ylamine (18.6 g) in toluene (185 ml) was added activated carbon (pH5 to 8, 9.29 g), and the mixture was stirred overnight under oxygen atmosphere at reflux. This reaction solution was cooled to room temperature, and then the activated carbon was filtered off through Celite, and eluted with ethyl acetate. This filtrate was concentrated under reduced pressure, the resulting residue was dissolved in toluene (185 ml), and to the solution was added fresh activated carbon (pH5 to 8, 9.29 g), and the mixture was stirred overnight under oxygen atmosphere at reflux. This reaction solution was cooled to room temperature, and then the activated carbon was filtered off through Celite, and eluted with ethyl acetate. This filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=4/1 to 1/1) to give the titled compound (8.68 g).

Fuente