反应详情

温度

60 °C

To a suspension of 3-cyclopropyl-1-((1-ethyl-1H-pyrazol-3-yl)methyl)-4-nitro-1H-indazole (7.55 g, 24.3 mmol) in EtOH/H2O (70 mL/15 mL) was added iron powder (27.1 g, 485 mmol) and NH4Cl (1.30 g, 24.3 mmol). The reaction mixture was heated to reflux for 3 hours. The mixture was cooled to 60° C. and filtered through a pad of Celite washing with a 20:1 EtOH/Et3N (300 mL) and 1:1 MeOH/DCM (300 mL). The filtrate was concentrated under reduced pressure. The residue was dissolved in EtOAc (300 mL), washed with saturated NaHCO3 solution, dried (Na2SO4) and concentrated under reduced pressure to give the product (7.1 g).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 3 hours
3. filtrationfiltered through a pad of Celite
4. washwashing with a 20:1 EtOH/Et3N (300 mL) and 1:1 MeOH/DCM (300 mL)
5. concentrationThe filtrate was concentrated under reduced pressure
6. dissolutionThe residue was dissolved in EtOAc (300 mL)
7. washwashed with saturated NaHCO3 solution
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated under reduced pressure