HRID489278

反应详情

EQUATION

反应方程式

HRID 489278 的结构方程式

CONDITIONS

反应条件

温度
102 °C

PROCEDURE

实验过程

1-Ethyl-3-cyano-5,6-dimethyl-2-pyridone (3-003-03) (3.37 g) was dissolved in 80% ethanol (65 mL), and to the reaction mixture was added potassium hydroxide (7.96 g), and the reaction mixture was refluxed with stirring in oil bath at 102° C. for 24 h. The reaction mixture was evaporated under reduced pressure, and to the residue were added water (50 mL) and ethyl acetate (50 mL). After the reaction mixture was stirred under ice-cooling, and was separated by shaking, and to the aqueous layer was conc. hydrochloric acid (13 mL). The resulting crystal was filtered, and washed with cooled water to give 1-ethyl-3-carboxy-5,6-dimethyl-2-pyridone (3-003-04) (2.734 g, 73.3%, m.p. 164-165° C.) as a yellow ocher crystal.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed
  2. customThe reaction mixture was evaporated under reduced pressure
  3. additionto the residue were added water (50 mL) and ethyl acetate (50 mL)
  4. stirringAfter the reaction mixture was stirred under ice-
  5. temperaturecooling
  6. customwas separated
  7. stirringby shaking
  8. filtrationThe resulting crystal was filtered
  9. washwashed with cooled water