This study aims at investigating the chemical constituents of Euphorbia hierosolymitana Boiss. Many compounds were isolated and characterized from this plant. One of them was characterized as a new one, 5-Aminopentyl (E)-3-(3, 4-dihydroxyphenyl) prop-2-enoate. Moreover, eleven other known compounds were identified, including: ursolic acid (2), oleanolic acid (3), 1-eicosanol (4), β-sitosteryl glucoside (5), quercetin (6), astragalin (7), eicosene (8), kaempferol-3,7-O-(α)-dirhamnoside (kaempferitrin) (9), quercetin-3-O-rhamnoside (10), myricitrin (11) and 1,2,3,4-tetra-O-galloyl-β-D-glucose (12). The structures of the isolated compounds were elucidated using spectroscopic techniques, such as UV, (1H,13C and 2D) NMR and HRESIMS. All compounds were isolated for the first time from this plant.