Reaktion #736392

ord-85ee90f0b41549cb94906eaf1651fe9d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture, refluxed for 10 hours
  2. 2
    Einengenconcentrated to dryness
  3. 3
    workup.ADDITIONTo the residue, were added ice-water (10 ml)
  4. 4
    Sonstigechloroform (100 ml) in this order, and the chloroform layer was separated
  5. 5
    Waschenwashed with water
  6. 6
    Sonstigedried
  7. 7
    Sonstigeevaporated
  8. 8
    SonstigeThe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04738975uspto-grants-1988_04