Reacción #11954

ord-556b3489715040888ff745b81e37a366

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroAfter the completion of the reaction
  2. 2
    Otrothe solid was removed
  3. 3
    Filtraciónfilter
  4. 4
    Concentraciónthe filtrate was concentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in chloroform
  6. 6
    Lavadowashed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine
  7. 7
    SecadoThe solution was dried over anhydrous sodium sulfate
  8. 8
    OtroThe solvent was removed by distillation
  9. 9
    Otrothe residue was dried under reduced pressure

Procedimiento

The compound obtained in Example 17-1 (269.9 mg) was dissolved in carbontetrachloride (8 ml), and N-bromosuccinimide (252.6 mg) and azobisisobutylonitrile (22.1 mg) were added to the solution. The mixture was stirred for 6 hours at 70° C. After the completion of the reaction, the solid was removed using a glass filter and the filtrate was concentrated. The residue was dissolved in chloroform and washed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine. The solution was dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was dried under reduced pressure to obtain the title compound (363.3 mg) as pale yellow oil.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07098215B2uspto-grants-2006_08