HRID1837339

反应详情

EQUATION

反应方程式

HRID 1837339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureis heated
  2. temperatureat reflux for 1.5 hours
  3. filtrationthen filtered hot through a pad of Diatomaceous earth
  4. washwashing with ethanol
  5. customthe precipitated solids are removed by filtration
  6. concentrationThe filtrate is concentrated to a small volume
  7. custompartitioned between ethyl acetate and water
  8. dry with materialThe organic layer is dried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo