Reacción #47908

ord-61a00e1c7bf64add85edd2fb46139082

Condiciones de reacción

Temperatura
150°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe solvents were removed under vacuum
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  3. 3
    Lavadowashed with sat. NaHCO3 and brine
  4. 4
    SecadoThe organic layer was dried over Na2SO4
  5. 5
    Filtraciónfiltered
  6. 6
    Otroevaporated
  7. 7
    Otroto give a brown residue
  8. 8
    OtroThe residue was purified

Procedimiento

N-(6-(Trifluoromethyl)pyridin-3-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (130 mg, 0.44 mmol) was dissolved in a mixture of dioxane/N,N-dimethylacetamide (4:1) (2 mL). To the mixture was added 2,3-dichloropyridine (98 mg, 0.66 mmol) and N,N-diisopropylethylamine (0.11 mL, 0.66 mmol). The mixture was heated at 150° C. in a Personal Chemistry microwave for 16 h. The solvents were removed under vacuum and the residue was dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give a brown residue. The residue was purified using a gradient of ethyl acetate:hexane (0-100%) to give the desired compound as an off-white powder (50 mg, 28%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07745451B2uspto-grants-2010_06