A series of monofluoro- and trifluoromethane-3,5-disubstituted 1,2,4-triazole compound was synthesized by using new efficient 1,3-dipolar cycloaddition method. This newly developed method was reaeacting hydrazonoyl hydrochlorides with a series of aldehydes in the presence of NEt3 as catalytic basic agent. The yielding cycloaddition products seemed not affect with the substituted on hydrazonoyl hydrochlorides. The preliminary asay d data indicate that some of of fluorine- and trifluoromethane-containing compounds can effectively be appbpJicable to inhibit ainst the growth of NCI-H226 and T-cell leukemia (Jurkat) two cells. In particular, trifluoromethane-containing 1,2,4-triazoles possessed the five membered ring groups on the C-5 position of triazolic ring, incuding cyclopentyl, 3-furyl, 3-thienyl, and 2-Pyrrolyl, possessed the significant inhibitory activity for NCI-H226.