Reacción #87409

ord-99a68e4d6adb4e8ab8a115ee8c7c5495

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGThe reaction was stirred at room temperature for 2.5 hours
  2. 2
    Extracciónthe mixture was extracted with ethylacetate
  3. 3
    LavadoThe organic phase was washed with water, brine
  4. 4
    Secadodried over magnesium sulfate
  5. 5
    Otrothe solvent was removed under reduced pressure
  6. 6
    OtroThe residue was purified by flash chromatography on silica gel
  7. 7
    Lavadoeluting with mixtures of 0% to 10% ethyl acetate in heptanes

Procedimiento

Sodium hydride (19.0 mg, 0.46 mmol) was added to a solution of cyclopropylmethanol (0.037 mL, 0.46 mmol) in dry THF (1 mL) at room temperature. The mixture was stirred for 5 minutes and then a solution of 2,4-dichloro-6-[(2,2,2-trifluoroethoxy)methyl]pyrimidine (120 mg, 0.46 mmol) in dry THF (1 mL) was added. The reaction was stirred at room temperature for 2.5 hours. Water was added and the mixture was extracted with ethylacetate. The organic phase was washed with water, brine, dried over magnesium sulfate and the solvent was removed under reduced pressure. The residue was purified by flash chromatography on silica gel, eluting with mixtures of 0% to 10% ethyl acetate in heptanes to afford the title compound as a solid, 40 mg, (29%) as yellow solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09439904B2uspto-grants-2016_09