HRID567881

反应详情

EQUATION

反应方程式

HRID 567881 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

7

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 2-bromophenol (380 mg) in N,N-dimenthylformamide (2.5 ml) were added potassium carbonate (15 mg), copper (19.5 mg), copper iodide, (15 mg) and 6-bromo-3,4-dimethoxyacetophenone (Compound 4) (130 mg) and the mixture was stirred at 100° C. for four hours. The reaction mixture was diluted with ether and 5% aqueous solution of sodium hydroxide was added thereto followed by stirring for five minutes. This was diluted with a mixture of ether and hexane and was washed with 5% aqueous solution of sodium hydroxide, water and saturated sodium chloride solution successively. The organic layer was collected and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom. The resulting residue was purified by a silica gel chromatography (hexane:ether=3:1) to give the title compound (345 mg, 80%) as yellow oil.

WORKUP

后处理

  1. additionwas added
  2. stirringby stirring for five minutes
  3. washwas washed with 5% aqueous solution of sodium hydroxide, water and saturated sodium chloride solution successively
  4. customThe organic layer was collected
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated
  7. customThe resulting residue was purified by a silica gel chromatography (hexane:ether=3:1)