HRID746824
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
- 65 °C
PROCEDURE
实验过程
To a solution of 2-(2-methoxy-4-nitrophenyl)pyridine (5.4 g, 23.3 mmol), dimethyl hydrazine (14 mL, 233 mmol), charcoal (0.7 g), in methanol (200 mL) was added iron trichloride (0.075 g, 0.46 mmol), then heated at 65° C. overnight. The reaction mixture was quenched with H2O (50 mL), then extracted with EtOAc (3×50 mL) and the combined organic extracts washed with brine. The organic phase was dried over Na2SO4 and concentrated in vacuo. The crude purified by liquid chromatography on silica (EtOAc/Hexane 3/7) to give 3-methoxy-4-pyridin-2-ylaniline.
WORKUP
后处理
- customThe reaction mixture was quenched with H2O (50 mL)
- extractionextracted with EtOAc (3×50 mL)
- washthe combined organic extracts washed with brine
- dry with materialThe organic phase was dried over Na2SO4
- concentrationconcentrated in vacuo
- customThe crude purified by liquid chromatography on silica (EtOAc/Hexane 3/7)