Reaktion #53579

ord-9aa8631c2eb64e40b3b9fd6dd9f8e030

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGAfter further 3 hours of stirring at room temperature
  2. 2
    WaschenThe organic layer was washed with water twice
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

6.7 g (22.0 mmol) of 4-(2,6-dichloro-4-trifluoromethylphenyl)toluene prepared in (a) was dissolved in 50 ml of chloroform, and 3.8 g (32.6 mmol) of chlorosulfonic acid was added dropwise at 0° C. with stirring. After further 3 hours of stirring at room temperature, the reaction mixture was poured into about 200 ml of ice-cold water for separation. The organic layer was washed with water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 7.2 g of 5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzenesulfonyl chloride (yield 81.0%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858639B2uspto-grants-2005_02