HRID468716

反应详情

EQUATION

反应方程式

HRID 468716 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. filtrationit was filtered through a celite pad
  3. customOrganic solvent was removed under reduced pressure, and it
  4. extractionwas extracted with CH2Cl2 (3×30 mL)
  5. dry with materialThe combined organic layer was dried over Na2SO4, and solvent
  6. customwas removed