Reaktion #75122

ord-9b77ae0b880f4839ae228a99d08f44fb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturUpon completion, the whole is heated
  2. 2
    Temperaturto reflux
  3. 3
    Temperaturat reflux temperature
  4. 4
    TemperaturAfter cooling
  5. 5
    Sonstigethe reaction mixture is evaporated
  6. 6
    Sonstigethe residue is crystallized from 2,2'-oxybispropane

Vorschrift

To a stirred mixture of 23 parts of 1,3-dihydro-1-(3-hydroxypropyl)-5-(trifluoromethyl)-2H-benzimidazol-2-one in 150 parts of trichloromethane are added dropwise 32 parts of sulfinyl chloride. Upon completion, the whole is heated to reflux and stirring is continued for 1 hour at reflux temperature. After cooling, the reaction mixture is evaporated and the residue is crystallized from 2,2'-oxybispropane, yielding 14 parts (56%) of 1-(3-chloropropyl)-1,3-dihydro-5-(trifluoromethyl)-2H-benzimidazol-2-one.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04175129uspto-grants-1979_11