Reaktion #4009

ord-c5c4f3d95a07449791cf3a5bbb4138ec

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter this time, the solution was cooled
  2. 2
    Sonstigeevaporated in vacuo
  3. 3
    SonstigeThe residue was partitioned between ethyl acetate and water
  4. 4
    Sonstigethe organic phase was separated
  5. 5
    Waschenwashed three times with water
  6. 6
    Trocknenthen dried (MgSO4)
  7. 7
    SonstigeEvaporation of the solvent
  8. 8
    Sonstigegave the crude product which
  9. 9
    Sonstigewas purified by chromatography on silica (Merck Kieselgel 60)
  10. 10
    Wascheneluted with ether

Vorschrift

3,56 Parts of 2-amino-4-chloro-6-chloromethylpyrimidine and 2.24 parts of potassium t-butoxide were dissolved in 60 parts of n-butanol at room temperature then the solution was heated at 50° C. for 2 hours, with stirring. After this time, the solution was cooled and evaporated in vacuo. The residue was partitioned between ethyl acetate and water and the organic phase was separated and washed three times with water then dried (MgSO4). Evaporation of the solvent gave the crude product which was purified by chromatography on silica (Merck Kieselgel 60) eluted with ether to give 2-amino-4-n-butoxy-6-chloromethylpyrmidine as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04723006uspto-grants-1988_02