HRID1708300

反应详情

EQUATION

反应方程式

HRID 1708300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-[4-(4-methoxyanilinocarbonyl)phenyl]-3,4-dihydrocarbostyril (0.2 g) in dimethylformamide (15 ml) is added 60% sodium hydride (24 mg) with stirring under ice cooling and the mixture is stirred at room temperature for 0.5 hour. Then, thereto is added a solution of ethyl bromide (64 mg) in dimethylformamide (DMF, 1 ml) and the mixture is refluxed with heating for 1 hour. DMF is distilled off under reduced pressure and water is added to the residue and the mixture is extracted with dichloromethane. The extract is washed with water and dried with magnesium sulfate. The solvent is distilled off under reduced pressure and the resulting residue is purified by silica gel column chromatography to give 1-[4-(N-ethyl-4-methoxyanilinocarbonyl)phenyl]-3,4-dihydrocarbostyril (0.12 g).

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature for 0.5 hour
  2. temperaturethe mixture is refluxed
  3. temperaturewith heating for 1 hour
  4. distillationDMF is distilled off under reduced pressure and water
  5. additionis added to the residue
  6. extractionthe mixture is extracted with dichloromethane
  7. washThe extract is washed with water
  8. dry with materialdried with magnesium sulfate
  9. distillationThe solvent is distilled off under reduced pressure
  10. customthe resulting residue is purified by silica gel column chromatography