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