HRID468716
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
- 75 °C
PROCEDURE
实验过程
To a solution of 3-bromo-2-methyl-5-nitropyridine (2.3 g, 10.5 mmol) in EtOH (20 mL) was added water (40 mL), NH4Cl (2.25 g, 42 mmol) and iron powder (2.94 g, 52.5 mmol). The mixture was stirred at 75° C. for 2 hours. After the reaction mixture was cooled to room temperature, it was filtered through a celite pad. Organic solvent was removed under reduced pressure, and it was extracted with CH2Cl2 (3×30 mL). The combined organic layer was dried over Na2SO4, and solvent was removed to give an off-white solid (1.52 g, 77%).
WORKUP
后处理
- temperatureAfter the reaction mixture was cooled to room temperature
- filtrationit was filtered through a celite pad
- customOrganic solvent was removed under reduced pressure, and it
- extractionwas extracted with CH2Cl2 (3×30 mL)
- dry with materialThe combined organic layer was dried over Na2SO4, and solvent
- customwas removed