HRID243190

反应详情

EQUATION

反应方程式

HRID 243190 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringwas stirred under an atmosphere of hydrogen at atmospheric pressure and 20° C. for 5 h
  2. customThe catalyst was removed by filtration
  3. concentrationconcentrated in vacuo
  4. customThe resulting residue was purified by chromatography (SiO2, 0-8% (2M ammonia in methanol) in DCM)