A new class of 1-substituted diazen-1-ium-1, 2-diolates (nitric oxide donors previously known as NONOates) were obtained by preparing esters of the naturally occurring polyamines putreanine (1) and spermic acid (2) with either cholesterol or hexadecanol. The syntheses of the following compounds and the corresponding NONOates are reported : cholesterylputreanine (5), dicholesterylspermate (6), hexadecanylputreanine (7), and dihexadecanylspermate (8).