HRID1857273

反应详情

EQUATION

反应方程式

HRID 1857273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6,7-Dimethoxy-4-(4-aminophenoxy)quinoline (53 mg) was dissolved in toluene (5 ml) with heat, after the addition of triethylamine (1 ml), triphosgene (101 mg) was added, and the admixture was ref luxed with heat for 4 minutes. 3,5-Dimethoxyaniline (62 mg) was added to the reaction mixture, and the admixture was refluxed with heat for 13 minutes. After the addition of aqueous sodium hydrogen carbonate, the reaction mixture was extracted 2 times with ethyl acetate, and the organic layer was then washed with brine and 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 (10/1) to obtain 85 mg of the title compound (yield: 100%)).

WORKUP

后处理

  1. temperaturewith heat
  2. additionwas added
  3. temperaturewith heat for 4 minutes
  4. temperaturethe admixture was refluxed
  5. temperaturewith heat for 13 minutes
  6. extractionthe reaction mixture was extracted 2 times with ethyl acetate
  7. washthe organic layer was then washed with brine
  8. dry with materialdried with anhydrous sodium sulfate
  9. customThe solvent was removed by reduced-pressure distillation
  10. customthe resulting residue was purified by column chromatography on silica gel eluting with chloroform/acetone (10/1)