Ethanol → 1-Ethyl-3-carboxy-5,6-dimethyl-2-pyridone

温度

102 °C

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.

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

ORDレコード

ord-f5cae6039413420dbd475217c3ecc5d6

出典データセット

uspto-grants-2005_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06977266B2