HRID546779

反应详情

EQUATION

反应方程式

HRID 546779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

2,6-Difluoro-3-nitropyridine (3.84 g) was dissolved in ethanol (42 ml). A solution of iron powder (4.03 g) and ammonium chloride (2.57 g) in water (14 ml) was added, and the reaction solution was heated and stirred at 80° C. for one hour. After leaving to cool, the reaction solution was filtered through celite. Ethyl acetate and water were added and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.06 g). The property values of the compound are as follows.

WORKUP

后处理

  1. temperaturethe reaction solution was heated
  2. customAfter leaving
  3. temperatureto cool
  4. filtrationthe reaction solution was filtered through celite
  5. additionEthyl acetate and water were added
  6. customthe organic layer was separated
  7. washThe resulting organic layer was washed with brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe drying agent was separated by filtration
  10. concentrationthe organic layer was concentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography