HRID1732484

反应详情

EQUATION

反应方程式

HRID 1732484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

p-Hydroxyacetophenone (13.6 g.), 1,3-dibromopropane (121.2 g.) and potassium carbonate (15.8 g.) were dissolved in acetone (250 ml.), and the solution was refluxed under heating for 6 hours. After the reaction mixture was filtered, the acetone was removed by evaporation from the filtrate under reduced pressure to give an oily residue. The excess of 1,3-dibromopropane was removed by distillation from the oily residue under reduced pressure to give a residue, which was subjected to column chromatography on silica gel (20 g.). Elution was carried out with benzene and the fractions containing a desired compound were collected. The eluate was evaporated to dryness under reduced pressure to give p-(3-bromopropoxy)acetophenone (18 g.).

WORKUP

后处理

  1. temperaturethe solution was refluxed
  2. temperatureunder heating for 6 hours
  3. filtrationAfter the reaction mixture was filtered
  4. customthe acetone was removed by evaporation from the filtrate under reduced pressure
  5. customto give an oily residue
  6. customThe excess of 1,3-dibromopropane was removed by distillation from the oily residue under reduced pressure
  7. customto give a residue, which
  8. washElution
  9. additionthe fractions containing a desired compound
  10. customwere collected
  11. customThe eluate was evaporated to dryness under reduced pressure