Reaktion #4794

ord-3d549740ce134666822d464aa2a445ae

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigen-propanol was evaporated off
  2. 2
    workup.ADDITIONTo the residue was added chloroform under ice-
  3. 3
    Temperaturcooling
  4. 4
    Sonstigeinsoluble materials were removed by means of celite filtration
  5. 5
    SonstigeFrom the resultant solution was removed chloroform
  6. 6
    Sonstigeby evaporation
  7. 7
    Waschenfollowed by elution with 10% methanol-chloroform

Vorschrift

To a solution of sodium n-propoxide solution prepared by dissolving sodium (1.7 g) in n-propanol (200 ml) was added to a hot solution of 2-methyl-4-nitropyridine-1-oxide (5.2 g) in n-propanol (210 ml). The mixture was stirred for ten minutes, then n-propanol was evaporated off. To the residue was added chloroform under ice-cooling, and insoluble materials were removed by means of celite filtration. From the resultant solution was removed chloroform by evaporation. The residue was subjected to a silica-gel column chromatography, followed by elution with 10% methanol-chloroform to yield 2-methyl-4-propoxypyridine-1-oxide (4.7 g) as an oily substance.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04727150uspto-grants-1988_02