Reacción #8473

ord-68e35b96105c48e0ba0ea364160d7487

Disolventes

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe mixture was cooled to ambient temperature
  2. 2
    Temperaturaheated
  3. 3
    Temperaturaat reflux temperature for 18 hours
  4. 4
    TemperaturaThe mixture was cooled to ambient temperature
  5. 5
    Otroevaporated to dryness
  6. 6
    OtroThe residue was crystallized

Procedimiento

The product of Step A (1.8 g) in dry acetonitrile (40 mL) was treated sequentially with tetrakis(triphenylphosphine)palladium(0) (0.1 g), triethylamine (1.27 g), and CuI (10 mg) then heated at 60° C. for 30 minutes. The mixture was cooled to ambient temperature, treated with 3-butyn-1-ol (0.361 g) and heated at reflux temperature for 18 hours. The mixture was cooled to ambient temperature and evaporated to dryness. The residue was crystallized, twice, from acetone to afford the title compound (1.02 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07087757B2uspto-grants-2006_08