A series of novel diquinazoline diselenide compounds was designed and synthesized with substituted 4-chloroquinazoline and sodium diselenide. Their structures were confirmed by IR, H-1 NMR, C-13 NMR, and elemental analyses. The antitumor activity of the new compounds was evaluated by MTT method. Compound 1a, 1c, 1h and 1i were found to have activities against MDA-MB-435, A549, MDA-MB-231, SiHa, and HeLa cells. Moreover, compared with the commercial anticancer drugs Gefitinib, Oxaliplatin, Taxol, 10-Hydroxycamptothecin, and Epirubicin Hydrochloride, la exerted better antitumor effects on corresponding cell lines at 10 mu M.