Реакция #442163

ord-22712608a2a94061928dadeb9849bf6a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture is cooled
  2. 2
    Другоеthe layers are separated
  3. 3
    ДругоеThe organic phase is dried
  4. 4
    Фильтрацияfiltered
  5. 5
    Другоеevaporated
  6. 6
    ДругоеThe residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
  7. 7
    ФильтрацияThe product is filtered off
  8. 8
    Другоеdried

Методика

A mixture of 4.9 parts of 1-(3-chloropropyl)-1H-benzimidazole, 5.76 parts of 1-[bis(4-fluorophenyl)methyl]piperazine, 5.3 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 20 hours with water-separator. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane. The product is filtered off and dried, yielding 1-[3-{4-[bis(4-fluorophenyl)methyl]-1-piperazinyl}propyl]-1H-benzimidazole hydrate; mp. 108.4° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04377578uspto-grants-1983_03