HRID582203

反应详情

EQUATION

反应方程式

HRID 582203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(3-Bromo-4-methoxyphenyl)propionic acid (5.0 g, 19.3 mmol) and thionyl chloride (10 ml) were refluxed for 1 hour. This reaction mixture was concentrated under reduced pressure to remove the excess thionyl chloride and the residue was dissolved in 1,2-dichloroethane (50 ml). To this solution was added aluminum chloride (2.8 g, 20.8 mmol) over 10 minutes on an ice bath and the mixture was further stirred at room temperature for 1 hour. This reaction mixture was poured in iced water and extracted with ethyl acetate. The extract was washed serially with saturated saline and water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was washed with hexane to provide the title compound (yield 4.3 g, 92%).

WORKUP

后处理

  1. concentrationThis reaction mixture was concentrated under reduced pressure
  2. customto remove the excess thionyl chloride
  3. dissolutionthe residue was dissolved in 1,2-dichloroethane (50 ml)
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed serially with saturated saline and water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. washThe residue was washed with hexane