Реакция #442165

ord-6d4cde76017b4b41a0b9325c0fc55f59

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
    ФильтрацияThe salt is filtered off
  7. 7
    Другоеcrystallized from 2-propanol

Методика

A mixture of 4.9 parts of 1-(3-chloropropyl)-1H-benzimidazole, 7 parts of 1-[(2-chlorophenyl)phenylmethyl]piperazine acetate, 10.6 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 converted into the hydrochloride salt in 2-propanol and 2,2'-oxybispropane. The salt is filtered off and crystallized from 2-propanol, yielding 1-[3-{4-[(2-chlorophenyl)phenylmethyl]-1-piperazinyl}propyl]-1H-benzimidazole trihydrochloride dihydrate; mp. 182.9° C.

Источник

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