HRID1837339
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
A mixture of 2-fluoro-1-(2-methoxyethoxy)-4-nitrobenzene (12.0 g , 55.7 mmol), iron powder (10.3 g, 180 mmol) and ammonium chloride (14.5 g , 270 mmol) in 170 mL of ethanol and 50 mL of water is heated at reflux for 1.5 hours then filtered hot through a pad of Diatomaceous earth, washing with ethanol. The filtrate is cooled to room temperature and the precipitated solids are removed by filtration. The filtrate is concentrated to a small volume and partitioned between ethyl acetate and water. The organic layer is dried over magnesium sulfate, filtered and concentrated in vacuo to provide 9.45 g of 3-fluoro-4-(2-methoxyethoxy)aniline as a brown liquid.
WORKUP
后处理
- temperatureis heated
- temperatureat reflux for 1.5 hours
- filtrationthen filtered hot through a pad of Diatomaceous earth
- washwashing with ethanol
- customthe precipitated solids are removed by filtration
- concentrationThe filtrate is concentrated to a small volume
- custompartitioned between ethyl acetate and water
- dry with materialThe organic layer is dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo