Reacción #87253

ord-9a61dfbe360d40bc9027ec867de0e0e5

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONwas added
  2. 2
    ConcentraciónThe solvent was concentrated under reduced pressure
  3. 3
    Otrothe reaction mixture was partitioned between EtOAc (50 mL) and H2O (50 mL)
  4. 4
    OtroThe organic layer was separated
  5. 5
    Extracciónthe aqueous layer extracted with EtOAc (50 mL)
  6. 6
    SecadoThe combined organics were dried over Na2SO4
  7. 7
    Filtraciónfiltered
  8. 8
    Concentraciónconcentrated under reduced pressure

Procedimiento

Dimethyl 5-hydroxyisophthalate (0.40 g, 1.90 mmol), cesium carbonate (1.30 g, 3.80 mmol) and CH3CN (12 mL) were added to a round-bottom flask and stirred for 15-30 min. iodobutane (0.42 g, 2.28 mmol) was added, and the reaction was stirred for 16 h. The solvent was concentrated under reduced pressure, and the reaction mixture was partitioned between EtOAc (50 mL) and H2O (50 mL). The organic layer was separated and the aqueous layer extracted with EtOAc (50 mL). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure to afford the desired product which was used without further purification.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09439433B2uspto-grants-2016_09