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In order to find new anticancer drugs, a series of novel furoxan-based coumarin derivatives (<i>10a</i>-<i>k</i>) were synthesized and evaluated for their antiproliferative activities in vitro. All compounds displayed more potent inhibition on human cervical cancer HeLa cell proliferation than coumarin-3-carboxylic acid, and compounds <i>10b</i>,<i> 10c</i>,<i> 10f</i>,<i> 10h</i>, and <i>10i</i> with IC<sub>50</sub> values ranging from 0.88 to 5.95 μM were even stronger than doxorubicin (IC<sub>50</sub> = 10.21 μM). The further study showed that compound <i>10i</i> exerted the highest antiproliferative activity (IC<sub>50</sub> = 0.60 μM) against human breast cancer MCF-7 cells, and compound <i>10f</i> had broader spectrum antiproliferative activity against five cancer cells with IC<sub>50</sub> values in the low micromolar range of 1.86-9.85 μM. More interestingly, compound <i>10f</i> had little effect on normal intestinal epithelial CCD841 cells. Our findings suggest that these novel furoxan-based coumarin derivatives may provide a new framework for the discovery of novel antitumor agents for the intervention of human carcinoma cells.