Reacción #75178

ord-27a702bd8f0947e69975d84c1df7a210

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Filtraciónthe catalyst is filtered off over hyflo
  2. 2
    Otrothe filtrate is evaporated
  3. 3
    OtroThe residue is crystallized from a mixture of 2-propanol and ethanol
  4. 4
    FiltraciónThe product is filtered off
  5. 5
    Otrodried

Procedimiento

A mixture of 64 parts of 5-chloro-1,3-dihydro-1-{1-[3-(2-nitrophenylamino)propyl]-4-piperidinyl}-2H-benzimidazol-2-one in 200 parts of methanol and 225 parts of tetrahydrofuran is hydrogenated at normal pressure and at room temperature with 10 parts of Raney-nickel catalyst. After the calculated amount of hydrogen is taken up, the catalyst is filtered off over hyflo and the filtrate is evaporated. The residue is crystallized from a mixture of 2-propanol and ethanol. The product is filtered off and dried, yielding 42 parts (70.5%) of 1-[1-{3-[N-(2-aminophenyl)amino]propyl}-4-piperidinyl]-5-chloro-1,3-dihydro-2H-benzimidazol-2-one; mp. 196° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04175129uspto-grants-1979_11