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
- 100 °C
PROCEDURE
实验过程
Iron (3.72 g) and ammonium chloride (7.13 g) were added to a solution of ethyl (E)-3-(6-methoxy-5-nitropyridin-2-yl)acrylate (2.1 g) in ethanol (100 mL) and water (20 mL). The reaction solution was stirred at 100° C. for one hour and then left to cool to room temperature. The reaction solution was filtered through celite. Ethyl acetate was added and the organic layer was separated. The resulting organic layer was washed with saturated sodium bicarbonate water and brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system) to obtain 1.85 g of the title compound. The property values of the compound are as follows.
WORKUP
后处理
- waitleft
- temperatureto cool to room temperature
- filtrationThe reaction solution was filtered through celite
- additionEthyl acetate was added
- customthe organic layer was separated
- washThe resulting organic layer was washed with saturated sodium bicarbonate water and brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)