Reacción #4009

ord-c5c4f3d95a07449791cf3a5bbb4138ec

Condiciones de reacción

Temperatura
50°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter this time, the solution was cooled
  2. 2
    Otroevaporated in vacuo
  3. 3
    OtroThe residue was partitioned between ethyl acetate and water
  4. 4
    Otrothe organic phase was separated
  5. 5
    Lavadowashed three times with water
  6. 6
    Secadothen dried (MgSO4)
  7. 7
    OtroEvaporation of the solvent
  8. 8
    Otrogave the crude product which
  9. 9
    Otrowas purified by chromatography on silica (Merck Kieselgel 60)
  10. 10
    Lavadoeluted with ether

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04723006uspto-grants-1988_02