Reaktion #74648

ord-fe75e3f41a77445d8b90cb62f7c10b93

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe organic layer was collected
  2. 2
    Waschenwashed with brine (20 mL)
  3. 3
    Trocknendried over sodium sulphate
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigeThe residue was triturated in dichloromethane
  6. 6
    Filtrationfiltered

Vorschrift

To a suspension of 2-iodo-4-(trifluoromethoxy)phenol (Preparation 226, 600 mg, 1.97 mmol) and potassium carbonate (1125 mg, 8.14 mmol) in Dimethylsulfoxide (10 mL) was added 3-cyano-4-fluoro-N-[1,2,4]thiadiazol-5-yl-benzenesulfonamide (Preparation 65). The reaction was heated to 80° C. under N2 for 7 hours before the addition of ethyl acetate (20 mL) and 3M aqueous HCl solution (30 mL). The organic layer was collected, washed with brine (20 mL), dried over sodium sulphate and concentrated in vacuo. The residue was triturated in dichloromethane and filtered to afford 965 mg of the title compound.

Quelle

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