HRID1190812

反应详情

EQUATION

反应方程式

HRID 1190812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

To a solution of 2,6-dichloro-4-nitropyridine (14.82 g, 76.79 mmol) in 350 mL ethanol were sequentially added iron powder (19.91 g, 356.58 mmol), water (65.8 mL, 3.6 mol) and concentrated hydrochloric acid (14.1 mL, 464.1 mmol). After the reaction was performed by stirring for 16 h at 95° C., the reaction solution was cooled to room temperature, adjusted to neutral pH, and subjected to suction filtration. After the filtrate was concentrated, it was extracted with ethyl acetate. The organic phase was combined, dried with anhydrous MgSO4, and subjected to rotary evaporation to afford 11.9 g titled product with a yield of 95.1%.

WORKUP

后处理

  1. temperaturethe reaction solution was cooled to room temperature
  2. filtrationsubjected to suction filtration
  3. concentrationAfter the filtrate was concentrated
  4. extractionit was extracted with ethyl acetate
  5. dry with materialdried with anhydrous MgSO4
  6. customsubjected to rotary evaporation