反应详情

A mixture of 1-benzyl-4-nitro-1H-indazole (150 mg; 0.592 mmol), iron powder (331 mg; 5.92 mmol) and ammonium chloride (16 mg; 0.296 mmol) in ethanol/water (4:1; 5 mL) was heated at reflux for 5 hours. The solvent was removed under vacuum and the residue was mixed with ethyl acetate/triethylamine (4:1; 5 mL) and heated at reflux for 1 hour. The mixture was allowed to cool and then filtered through a pad of silica, washing with ethyl acetate. The solvent was removed under vacuum to give the desired product that was used directly in the next step.

1. temperaturewas heated
2. temperatureat reflux for 5 hours
3. customThe solvent was removed under vacuum
4. additionthe residue was mixed with ethyl acetate/triethylamine (4:1; 5 mL)
5. temperatureheated
6. temperatureat reflux for 1 hour
7. temperatureto cool
8. filtrationfiltered through a pad of silica
9. washwashing with ethyl acetate
10. customThe solvent was removed under vacuum