反应详情

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).

1. temperatureat reflux
2. filtrationthe activated carbon was filtered off through Celite
3. washeluted with ethyl acetate
4. concentrationThis filtrate was concentrated under reduced pressure
5. dissolutionthe resulting residue was dissolved in toluene (185 ml)
6. additionto the solution was added fresh activated carbon (pH5 to 8, 9.29 g)
7. stirringthe mixture was stirred overnight under oxygen atmosphere
8. temperatureat reflux
9. temperatureThis reaction solution was cooled to room temperature
10. filtrationthe activated carbon was filtered off through Celite
11. washeluted with ethyl acetate
12. concentrationThis filtrate was concentrated under reduced pressure
13. customthe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=4/1 to 1/1)