In addition to phenolic constituents such as apigenin, quercetin, methyl gallate, gallic acid, and apigenin 7-O-beta-D-glucopyranoside, the leaves of Euphorbia thymifolia Burm. (Euphorbiaceae) were found to contain asperglaucide (1), aurantiamide (2), beta-sitosterol 3-O-beta-D-glucopyranoside (3), and luteolin-7-O-beta-D-glucopyranoside (4) in the present study. Their structures were determined by using MS, 1D and 2D NMR techniques.