HRID1648587

反应详情

EQUATION

反应方程式

HRID 1648587 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-(2,4-dimethoxybenzoylamino)phenyl]-3,4-dihydrocarbostyril (0.19 g) in dimethylformamide (8 ml) is added with stirring 60 % sodium hydride (0.02 g) under ice cooling. The mixture is stirred at room temperature for 0.5 hour and thereto is added a solution of methyl iodide (0.08 g) in dimethylformamide (6 ml). The mixture is stirred at room temperature for 3 hours. The solvent is distilled off under reduced pressure and water is added to the residue. The mixture is extracted with dichloromethane, 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-(2,4-dimethoxybenzoyl)-N-methylamino]phenyl)-3,4-dihydrocarbostyril (70 mg).

WORKUP

后处理

  1. stirringThe mixture is stirred at room temperature for 3 hours
  2. distillationThe solvent is distilled off under reduced pressure and water
  3. additionis added to the residue
  4. extractionThe mixture is extracted with dichloromethane
  5. washwashed with water
  6. dry with materialdried with magnesium sulfate
  7. distillationThe solvent is distilled off under reduced pressure
  8. customthe resulting residue is purified by silica gel column chromatography