反応 #75122

ord-9b77ae0b880f4839ae228a99d08f44fb

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度Upon completion, the whole is heated
  2. 2
    温度to reflux
  3. 3
    温度at reflux temperature
  4. 4
    温度After cooling
  5. 5
    その他the reaction mixture is evaporated
  6. 6
    その他the residue is crystallized from 2,2'-oxybispropane

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04175129uspto-grants-1979_11