Phytochemical studies on the leaves of Ailanthus altissima (Simaroubaceae) have not been reported previously. Thus, the authors isolated and identified secondary metabolites from A. altissima. Dried and powdered leaves were extracted with 80% aqueous methanol, and the concentrated extract was successively partitioned with ethyl acetate, n-butanol, and water. Four flavonoids were isolated from the ethyl acetate fraction through repeated silica gel and octadecyl silica gel column chromatography. Spectroscopic data including NMR, MS, and IR allowed for identification of the chemical structures as quercetin (1), afzelin (2), quercitrin (3), and isoquercitrin (4). This is the first report of the isolation of these compounds from A. altissima. The four isolated flavonoids 1-4 as well as solvent fractions (ethyl acetate, n-butanol, and water), were evaluated for DPPH radical scavenging activity.