Реакция #75148

ord-0b20b498803e49308aa1de366ef75836

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураrefluxed overnight
  2. 2
    ФильтрацияThe undissolved product is filtered off
  3. 3
    Другоеpurified by column-chromatography over silica gel using
  4. 4
    workup.ADDITIONa mixture of trichloromethane and 10% of methanol as eluent
  5. 5
    ДругоеThe pure fractions are collected
  6. 6
    Другоеthe eluent is evaporated

Методика

A mixture of 2.3 parts of 1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 2.31 parts of 1-phenyl-1,3,8-triazaspiro-[4,5]decan-4-one, 3.2 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling to room temperature, water is added. The undissolved product is filtered off and purified by column-chromatography over silica gel using a mixture of trichloromethane and 10% of methanol as eluent. The pure fractions are collected and the eluent is evaporated, yielding 0.9 parts (22%) of 8-[3-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one; mp. 228° C.

Источник

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