Reacción #633962

ord-baa37e6433c247bc9d522fbb5ae9a100

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas maintained at room temperature
  2. 2
    workup.STIRRINGThe reaction solution was further stirred at room temperature for four hours
  3. 3
    Otrothe organic layer was separated
  4. 4
    LavadoThe resulting organic layer was washed with brine
  5. 5
    Secadodried over anhydrous sodium sulfate
  6. 6
    OtroThe drying agent was separated by filtration
  7. 7
    Concentraciónthe organic layer was concentrated under reduced pressure
  8. 8
    OtroThe residue was purified by silica gel column chromatography

Procedimiento

Acetic anhydride (6 ml) was added to formic acid (6 ml), followed by stirring at room temperature for 20 minutes. Then, a solution of 2,6-difluoro-3-aminopyridine (2.06 g) in tert-butyl methyl ether (7 ml) was added so that the reaction solution was maintained at room temperature. The reaction solution was further stirred at room temperature for four hours. Ethyl acetate and a saturated sodium bicarbonate solution were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.42 g). The property values of the compound are as follows.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07935815B2uspto-grants-2011_05