Column chromatographic separation of the MeOH extract from the aerial parts of Hibiscus manihot led to the isolation of four compounds. Their structures were characterized to be hentriacontane (1), palmitic acid (2), daucosterol (3) and 3-dihydrocaffeonyl-5-p-coumaroylquinic acid (4) by spectroscopic methods. The compounds (1~4) were for the first time reported from this plant. The solvent fractions were tested for their antioxidant activities by free radical scavenging and superoxide dismutase (SOD).