HRID1023916
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
PROCEDURE
实验过程
To a stirred solution of 3-(4-ethyl-2-methoxyphenoxy)-2-nitropyridine (1.3 g, 4.7 mmol) in methanol (30 ml) were added anhydrous Ferric chloride (66 mg) and activated charcoal (66 mg). The resulting mixture was heated to reflux and Hydrazine hydrate (80%) (2 mL, 39 mmol) was added dropwise. The reaction was allowed to stir under reflux condition for 5 hours, then filtered through celite. The filtrate was concentrated under reduced pressure, taken in ethyl acetate (150 ml). The organic phase was washed with water followed by brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 1.11 g of the title compound, 100% yield.
WORKUP
后处理
- temperatureThe resulting mixture was heated
- temperatureto reflux
- temperatureunder reflux condition for 5 hours
- filtrationfiltered through celite
- concentrationThe filtrate was concentrated under reduced pressure
- washThe organic phase was washed with water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure