Abstract N-Monosubstituted 1, 3-diamines were selectively functionalized at the secondary N-atom via 2-Ph-substituted hexahydropyrimidine intermediates. Reaction of the diamines with benzaldehyde, followed by treatment with an electrophile and hydrolysis, provided the desired products with excellent selectivity and in high yields. N 4, N 9-bis [3-phenylprop-2- enoyl] spermine (4a), which was further converted to N 1, N 1 2-bis [3-phenylprop-2-enoyl] ...