Ten styrylquinoline derivatives were prepared from anilines and aromatic aldehydes in two steps. Firstly, four 2 -methylquinolines have been synthesized from anilines and (E)-2-butenal using hydrochloric acid as catalyst. Then styrylquinolines were obtained with 64% ~ 78% yield by refluxing 2-methylquinolines and aromatic aldehydes in glacial acetic acid. The structures of all synthesized compounds were confirmed by 1HNMR, MS and IR. The antitumor activity of these compounds against A 549 and HCT 116 cell lines was evaluated by MTT assay in vitro. The results showed that compounds Ⅱc exhibited high activity against A 549 and HCT 116 cell lines with IC50 value of 9.77 and 9.66 μmol·L-1, respectively, and compounds Ⅱd exhibited high activity against HCT 116 cell lines with IC50 value of 9.80 μmol·L-1 .