反应详情

温度

80 °C

To 3-iodo-1-((1-(4-methoxybenzyl)-1H-pyrazol-4-yl)methyl)-4-nitro-1H-indazole (1.13 g, 2.31 mmol) in EtOH/H2O (20 mL/5 mL) was added iron (1.29 g, 23.1 mmol) and NH4Cl (0.124 g, 2.31 mmol). The reaction mixture was heated to 80° C. and stirred for 3 hours. The reaction mixture was concentrated, diluted with EtOAc (30 mL) and Et3N (5 mL). The reaction mixture was heated to reflux for 30 minutes and filtered through Celite®, and the filter pad was washed with DCM/MeOH (50 mL, 10:1). The filtrate was concentrated to provide the desired product (0.89 g).

1. concentrationThe reaction mixture was concentrated
2. additiondiluted with EtOAc (30 mL) and Et3N (5 mL)
3. temperatureThe reaction mixture was heated
4. temperatureto reflux for 30 minutes
5. filtrationfiltered through Celite®
6. washthe filter pad was washed with DCM/MeOH (50 mL, 10:1)
7. concentrationThe filtrate was concentrated