Reaktion #523986

ord-f69818a69ece405a9de8fcb5e92ee636

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxed for 8 hr
  2. 2
    EinengenThe reaction mixture was concentrated
  3. 3
    Sonstigeto remove methyl alcohol, and water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    ExtraktionThe solution was extracted with n-hexane
  6. 6
    Trocknenthe n-hexane solution was dried over sodium sulfate
  7. 7
    EinengenThe dried n-hexane solution was concentrated
  8. 8
    workup.DISTILLATIONthe residue was distilled

Vorschrift

Sodium (92 mg) was dissolved in 5 ml of absolute methyl alcohol with moderate cooling. To this solution 2-hydroxypyrazolo[1,5-a]pyridine (500 mg) was added and then dimethyl sulfate (500 mg) was added. The mixture was stirred for 30 min. at room temperature and refluxed for 8 hr. The reaction mixture was concentrated to remove methyl alcohol, and water was added to the residue. The solution was extracted with n-hexane, and the n-hexane solution was dried over sodium sulfate. The dried n-hexane solution was concentrated and the residue was distilled to give 280 mg of oily product under reduced pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04028370uspto-grants-1977_06