Reacción #5000

ord-bef430985b434ffd803e950af8b3d2e0

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGThe mixture was stirred at 80° C. for 1 hour
  2. 2
    Temperaturaafter cooling
  3. 3
    OtroAn oily product thus precipitated
  4. 4
    Extracciónwas extracted with ethyl acetate
  5. 5
    Secadowas dried with magnesium sulfate anhydride
  6. 6
    workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
  7. 7
    Otrothe residue thus obtained
  8. 8
    Otrowas purified by column chromatography

Procedimiento

13.8 g of potassium carbonate and 50 ml of DMF were placed in a 200 ml eggplant type flask, and 11.1 g of methyl 2-formyl-6-hydroxybenzoate and 14.6 g of 4,6-dimethoxy-2-methanesulfonylpyrimidine were added thereto with stirring. The mixture was stirred at 80° C. for 1 hour, and the resultant liquor was poured into an ice water after cooling. An oily product thus precipitated was extracted with ethyl acetate, and was dried with magnesium sulfate anhydride. Ethyl acetate was distilled off under reduced pressure, and the residue thus obtained was purified by column chromatography to obtain 11.0 g of the aimed compound (melting point=91° to 93° C.) at a yield of 52%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05242895uspto-grants-1993_09