Reaktion #736392
ord-85ee90f0b41549cb94906eaf1651fe9d
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturthe mixture, refluxed for 10 hours
- 2Einengenconcentrated to dryness
- 3workup.ADDITIONTo the residue, were added ice-water (10 ml)
- 4Sonstigechloroform (100 ml) in this order, and the chloroform layer was separated
- 5Waschenwashed with water
- 6Sonstigedried
- 7Sonstigeevaporated
- 8SonstigeThe residue was purified by column chromatography on silica gel
Vorschrift
To a solution of 4-chloro-3-methoxy-2-methylpyridine (3.2 g) in methanol (5 ml) was added dropwise under ice-cooling a solution of 28% sodium methylate in methanol (20 ml) and the mixture, refluxed for 10 hours, and concentrated to dryness. To the residue, were added ice-water (10 ml) and then chloroform (100 ml) in this order, and the chloroform layer was separated, washed with water, dried, and evaporated. The residue was purified by column chromatography on silica gel, to give 3,4-dimethoxy-2-methylpyridine (2.95 g) as a light brown oil.