HCID 131719610, compound → HCID 131719609, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of the product of step (i) (5 g) and conc. HCl (50 ml) was heated at 100° C. for 45 min. The resultant solution was evaporated to dryness and the residue dissolved again in conc. HCl and heated to 100° C. for a further 45 min. The reaction mixture was evaporated to dryness, and the residue was twice triturated with toluene, and evaporated to dryness, collected and washed with ether. The crude product was crystallised from hot methanol/ether to give 4-[(4-pyridyl)piperazin-1-yl]butyric acid, dihydrochloride as an off-white crystalline solid (3.45 g): m.p. 280°-300° C. (dec); NMR (d6 -DMSO) δ2.00 (2H, m), 2.36 (2H, t), 3.12 (2H, m), 3.00-3.70 (4H, v. br, m), 3.50-4.50 (4H, v. br, m), 7.30 (2H, d), 8.35 (2H, d), 12.2 (1H, v. br); m/Z 250 (M+H)+ ; calculated for C13H19N3O2. 2.0 HCl. 0.5 H2O: C, 47.1%; H, 6.69%; N, 12.7%; found: C, 47.5%; H, 6.7%; N, 12.5%

Provenance & Evidence