反应详情

温度

85 °C

To a reaction flask was added 1-benzyl-3-cyclopropyl-4-nitro-1H-indazole (60.0 mg, 0.205 mmol), iron powder (114 mg, 2.05 mmol) and ammonium chloride (10.9 mg, 0.205 mmol). Ethanol (0.8 mL) and water (0.2 mL) were added and the mixture was heated at 85° C. with stirring for 60 minutes. The solvent was removed under reduced pressure. Ethyl acetate (0.8 mL) and triethylamine (0.2 mL) was added and the mixture was heated at 60° C. for 10 minutes. The mixture was filtered through glass fiber filter paper, washing with methanol and ethyl acetate. The filtrate was concentrated under reduced pressure. The material was purified by preparative chromatography, eluting with 3% methanol in dichloromethane, containing 0.5% ammonium hydroxide solution to give 1-benzyl-3-cyclopropyl-1H-indazol-4-amine (36 mg).

1. customThe solvent was removed under reduced pressure
2. additionEthyl acetate (0.8 mL) and triethylamine (0.2 mL) was added
3. temperaturethe mixture was heated at 60° C. for 10 minutes
4. filtrationThe mixture was filtered through glass fiber
5. filtrationfilter paper
6. washwashing with methanol and ethyl acetate
7. concentrationThe filtrate was concentrated under reduced pressure
8. customThe material was purified by preparative chromatography
9. washeluting with 3% methanol in dichloromethane
10. additioncontaining 0.5% ammonium hydroxide solution