Reaktion #74567

ord-b825268082ba4067a69655ff911ac4af

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with 1N HCl
  2. 2
    TrocknenThe organic layer was dried over sodium sulfate
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated
  5. 5
    SonstigeThe residue was purified by flash column chromatography

Vorschrift

To a slurry of 2-aminothiazole (23.88 g, 0.2384 mol) in methylene chloride (150 mL) and pyridine (38.0 mL, 0.470 mol) was added dropwise a solution of 3,4-difluorobenzenesulphonyl chloride (25.0 g, 0.118 mol) in 10 mL of methylene chloride. After stirring for 48 hours the reaction was diluted with more dichloromethane and extracted with 1N HCl. The organic layer was dried over sodium sulfate, filtered, and concentrated. The residue was purified by flash column chromatography to give 3,4-difluoro-N-(thiazol-2-yl)benzenesulfonamide as a white solid. LCMS Rt=1.24 minutes MS m/z 277 [MH]+

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541588B2uspto-grants-2013_09