Novel solanesylpiperazinotriamines as well as their N-aryl-substituted analogs were synthesized starting from solanesol through a multistep procedure. Their structures were confirmed by IR, (1)H NMR, MS, and elemental analysis. The preliminary results indicated that these novel derivatives were preferentially toxic against tumor cells, and at non-cytotoxic concentration, the synergistic effect of solanesyltriamines (3a and 3c) was even superior to that of N,N'-bis(3,4-dimethoxybenzyl)-N-solanesylethylenediamine. Interestingly, the cytotoxicity of solanesylpiperazinotriamine derivatives was markedly enhanced when conjugating with aryl pharmacophores (7-9).