Squamocin (I) was isolated from the seeds of Annona spinescens, the bark of Annona salzmanii, and the seeds of Annona atemoya, and was dried by azeotropic distillation with toluene. Glycosylation with pentaacetyl-alpha-D-glucopyranose (II) in the presence of boron trifluoride etherate produced a mixture of the target 15,24-diacetyl-28-(tetraacetyl-beta-D-glucosyl)squamocin and three other acetylated glucosides, which were separated by means of centrifugal partition chromatography.