Reacción #2193

ord-854622046616431a8dec648c46bb4905

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaunder reflux
  2. 2
    Concentraciónconcentrated
  3. 3
    workup.ADDITIONWater was added to the residue
  4. 4
    Extracciónthe mixture was extracted with ethyl acetate
  5. 5
    LavadoThe ethyl acetate layer was washed with water
  6. 6
    Secadodried over anhydrous magnesium sulfate
  7. 7
    Concentraciónconcentrated
  8. 8
    OtroThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1)

Procedimiento

4-chloro-4'-mercaptomethylbenzophenone (16.0 g), ethyl bromide (7.4 g) and potassium hydroxide (4.3 g) were added to methanol (250 ml), and the mixture was stirred for 30 minutes under reflux. The reaction mixture was cooled to room temperature and then concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1) to obtain the desired product 14.0 g, melting point: 33° to 34° C., yield: 79%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05728699uspto-grants-1998_03