EtOH extracts of Petalostemum purpureum demonstrated antimicrobial activity against bacteria and fungi. Bioassay-directed fractionation led to the isolation of petalostemumol [1] as the active constituent. Its structure was determined by a single crystal X-ray diffraction analysis. A minor component designated petalostemumol G [3] is believed to be an artifact of the isolation procedure. Its structure was confirmed by a single crystal X-ray analysis of its pentamethylether 2. A number of derivatives of 1 and 3, including the Me- and benzylethers and acetates, were prepared.