Reaktion #1508732

ord-ae7b094ee77040a8bb97d34f87210c1d

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationAfter the precipitated crystals were filtered off
  2. 2
    Waschenthe filtrate was successively washed with aquous sodium bicarbonate solution, aqueous 5% sodium thiosulfate solution and water
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONAfter distilling off the solvent
  5. 5
    Sonstigethe crude product was purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:5)

Vorschrift

4-Chloro-4'-methylsulfinylmethylbenzophenone (2.9 g) and m-chloroperbenzoic acid (2.5 g) were dissolved in dichloromethane, and the mixture was stirred for 12 hours at 0° C. After the precipitated crystals were filtered off, the filtrate was successively washed with aquous sodium bicarbonate solution, aqueous 5% sodium thiosulfate solution and water, and dried over anhydrous magnesium sulfate. After distilling off the solvent, the crude product was purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:5) to obtain 4-chloro-4'-methylsulfonylmethylbenzophenone (1.8 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06077866uspto-grants-2000_06