反応 #736392

ord-85ee90f0b41549cb94906eaf1651fe9d

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture, refluxed for 10 hours
  2. 2
    濃縮concentrated to dryness
  3. 3
    workup.ADDITIONTo the residue, were added ice-water (10 ml)
  4. 4
    その他chloroform (100 ml) in this order, and the chloroform layer was separated
  5. 5
    洗浄washed with water
  6. 6
    その他dried
  7. 7
    その他evaporated
  8. 8
    その他The residue was purified by column chromatography on silica gel

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04738975uspto-grants-1988_04