HCID 178441630, compound → HCID 178441633, compound

Participants

Reaction Steps

Under a static nitrogen atmosphere 2.30 g (4.5 mmol) of 5-[4′-[[3-(N-Boc-3-aminopropyl)-5-butyl-1H-1,2,4-triazol-1-yl]methyl][1,1′-biphenyl]-2-yl]-1H-tetrazole from Example 68 was dissolved in 30 mL of 4N HCl in dioxane at ambient temperature and allowed to stir overnight. The solvents were removed in vacuo; the residue was triturated with diethyl ether and filtered providing 1.99 g (98%) of 5-[4′-[[3-(3-aminopropyl)-5-butyl-1H-1,2,4-triazol-1-yl]methyl] (1,1′-biphenyl)-2-yl]-1H-tetrazole as the hydrochloride salt: NMR (DMSO-d6) δ 0.85 (t, J=7 Hz, 3H), 1.22–1.38 (m, 2H), 1.59 (t, J=8 Hz, 2H), 1.96 (t, J=8 Hz, 2H), 2.71–2.79 (m, 2H) 2.80–2.92 (m, 4H), 5.40 (s, 2H) 7.10 (d, J=8 Hz, 2H), 7.18 (d, J=8 Hz, 2H) 7.52 (d, J=8 Hz, 1H), 7.59 (d, J=8 Hz, 1H), 7.68 (d, J=8 Hz, 2H); MS (FAB) m/e (rel intensity) 417 (60), 389 (10), 357 (10), 263 (5), 235 (10), 207 (100), 166 (40), 136 (15); HRMS. Calc'd for M+H: 417.2515. Found: 417.2510.

Provenance & Evidence