Ammonia → HCID 70364112, compound

Participants

Reaction Steps

A mixture of 5 parts of N"-cyano-N-(2,2-dimethoxyethyl)-N'-[2-[4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]amino]-1-piperidinyl]ethyl]guanidine and 60 parts of concentrated hydrochloric acid was stirred and refluxed for one hour. Water was added and the whole was alkalized with ammonia. The product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) saturated with ammonia, as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from a mixture of acetonitrile and 2,2'-oxybispropane, yielding 1 part of N-[1-[2-(2-amino-1H-imidazol-1yl]ethyl]-4-piperidinyl]-1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-amine monohydrate; mp. 171.4° C. (compound 60).

Provenance & Evidence