反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturethe reaction mixture was refluxed
- customThe reaction mixture was evaporated under reduced pressure
- additionto the residue were added water (50 mL) and ethyl acetate (50 mL)
- stirringAfter the reaction mixture was stirred under ice-
- temperaturecooling
- customwas separated
- stirringby shaking
- filtrationThe resulting crystal was filtered
- washwashed with cooled water