Reacción #42738

ord-fa224b4cc0cd49ce92d0db54d17f8641

Disolventes

Condiciones de reacción

Temperatura
140°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe reaction mixture is cooled to room temperature
  2. 2
    workup.ADDITIONpoured onto ice-water
  3. 3
    Extracciónextracted with methylene chloride
  4. 4
    LavadoThe organic layer is washed with saturated sodium hydrogen carbonate solution
  5. 5
    Secadodried over anhydrous magnesium sulfate
  6. 6
    Otroevaporated to dryness in vacuo

Procedimiento

A mixture of 2-(4-chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione (3.65 g, 10.3 mmol) in acetic acid (36 ml) and concentrated HCl solution (2 ml) is stirred at 140° C. for 3 h. The reaction mixture is cooled to room temperature, poured onto ice-water and extracted with methylene chloride. The organic layer is washed with saturated sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate and evaporated to dryness in vacuo to afford the title compound as a brown solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07732435B2uspto-grants-2010_06