HRID1857147

反应详情

EQUATION

反应方程式

HRID 1857147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6,7-Dimethoxy-4-(4-aminophenoxy)quinoline (52 mg) was suspended in triethylamine/methylene chloride (3 ml/2 ml), commercially available biphenylcarbonyl chloride (80 mg) was added, and the admixture was stirred at room temperature for 25 hours. Aqueous sodium hydrogen carbonate was added to the reaction mixture, and the resulting admixture was extracted with ethyl acetate. The ethyl acetate layer was washed with brine and then dried with anhydrous sodium sulfate. The solvent was removed by reduced-pressure distillation, and the resulting residue was purified by column chromatography on silica gel eluting with chloroform/acetone and further by washing resulting crystals with acetoneto obtain 9 mg of the title compound (yield: 10%).

WORKUP

后处理

  1. extractionthe resulting admixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with brine
  3. dry with materialdried with anhydrous sodium sulfate
  4. customThe solvent was removed by reduced-pressure distillation
  5. customthe resulting residue was purified by column chromatography on silica gel eluting with chloroform/acetone
  6. washfurther by washing
  7. customresulting crystals with acetoneto