反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
A mixture of (5-fluoro-2-nitrophenyl)-(1-methyl-1H-pyrazol-4-yl)amine (102 mg, 0.43 mmol) and 10% palladium on carbon (25 mg) in EtOAc (10 mL) was stirred under an atmosphere of hydrogen at atmospheric pressure and 20° C. for 6 h. A separate mixture of (5-fluoro-2-nitrophenyl)-(1-methyl-1H-pyrazol-4-yl)amine (0.19 g, 0.80 mmol) and 10% palladium on carbon (50 mg) in EtOAc (10 mL) was stirred under an atmosphere of hydrogen at atmospheric pressure and 20° C. for 5 h. The catalyst was removed by filtration and the filtrates combined and concentrated in vacuo. The resulting residue was purified by chromatography (SiO2, 0-8% (2M ammonia in methanol) in DCM) to give the title compound as a brown oil (0.188 g, 74%). LCMS (Method C): RT 1.61 min [M+H]+ 207.1
WORKUP
后处理
- stirringwas stirred under an atmosphere of hydrogen at atmospheric pressure and 20° C. for 5 h
- customThe catalyst was removed by filtration
- concentrationconcentrated in vacuo
- customThe resulting residue was purified by chromatography (SiO2, 0-8% (2M ammonia in methanol) in DCM)