Реакция #75165

ord-b111eb825c164fc6955e28140acaddf3

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling
  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
    Другоеdried

Методика

A mixture of 3.58 parts of 1-(3-chloropropyl)-1,3-dihydro-5,6-dimethyl-2H-benzimidazol-2-one, 3.17 parts of 4-(4-chlorophenyl)-4-piperidinol, 5.3 parts of sodium carbonate, 0.2 parts of potassium iodide and 160 parts of 4-methyl-2-pentanone is stirred and refluxed for 24 hours with water-separator. After cooling, 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 methanol and 2-propanol. The salt is filtered off and dried, yielding 1.7 parts of 1-{3-[4-(4-chlorophenyl)-4-hydroxy-1-piperidinyl]propyl}-1,3-dihydro-5,6-dimethyl-2H-benzimidazol-2-one hydrochloride; mp. 260.8° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04175129uspto-grants-1979_11