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
- 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
- temperaturethe reaction solution was heated
- customAfter leaving
- temperatureto cool
- filtrationthe reaction solution was filtered through celite
- additionEthyl acetate and water were added
- customthe organic layer was separated
- washThe resulting organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- customThe drying agent was separated by filtration
- concentrationthe organic layer was concentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography