Hydrogen Bromide → HCID 86750399, compound

Participants

Reaction Steps

A mixture of (±)-ethyl 4-[4-[2-[1-(4-chlorobenzoyl)propyl]-2,3-dihydro-3-oxo-4H-1,2,4-triazol-4-yl]phenyl]-1-piperazinecarboxylate (15 g) in a hydrobromic acid solution 48% in water (150 ml) was stirred and refluxed or 6 hours and then stirred overnight. The mixture was evaporated, the residue was dissolved in CH2Cl2 and washed with NaHCO3 /H2O. The organic layer was dried, filtered and the solvent evaporate&. The residue was dissolved in 2-propanol and crystallized into the hydrochloric acid salt (1:2) in 2-propanol. The precipitate was filtered off and recrystallized from CH3CN, yielding 7.9 g (2.2%) of (±)-2-[1-(4-chlorobenzoyl)propyl]-2,4-dihydro-4-[4-(1-piperazinyl)phenyl]-3H-1,2,4-triazol-3-one . dihydrochloride . monohydrate; mp. 175.9° C. (interm. 1).

Provenance & Evidence