HRID428137

反应详情

EQUATION

反应方程式

HRID 428137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(E)-N-(3-hydroxyphenethyl)-3-(3-pyridyl)-2-propenoic acid amide (600 mg, 2.24 mmol) obtained in Example 81 was dissolved in pyridine (4.0 ml) and acetic anhydride (0.40 ml, 4.24 mmol) was added under ice-cooling and stirred at room temperature for 1.5 hours. Ethyl acetate was added to the reaction mixture and the mixture was washed with water and dried over magnesium sulfate. The solvent was distilled out under reduced pressure, and the residue was purified by silica gel column chromatography (methanol:dichloromethane=1:30) and recrystallized to yield the titled compound (574 mg, 82%).

WORKUP

后处理

  1. temperaturecooling
  2. washthe mixture was washed with water
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was distilled out under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (methanol:dichloromethane=1:30)
  6. customrecrystallized