Natural spinasterol-glucose (3-O-β-D-glucopyanosylspinasterol), isolated from Stewartia koreana leaves, has been identified as a compound to exhibit a potent anti-inflammatory activity. Further biological investigation with spinasterol glycosides was needed, but due to the difficulty and inefficiency of isolation and synthesis of natural spinasterol and other sterols it has not been done. In this study, we have prepared stigmasterol, spinasterol, schottenol, dihydroergosteol and ergosteol. ergostenol and their 3-epimers to test for the anticancer activity.