In addition to a previous report, the reaction of tigogenin acetate with ICl in refluxing CHCl 3 produced the hitherto unknown 23R-iodotigogenin acetate, bearing an axial iodine atom at C-23 and its already reported 23S-epimer. The same treatment of sarsasapogenin acetate led to a single diasteromer characterized as 23S-iodosarsasapogenin acetate. A full characterization of the obtained compound including 1 H, 13 C NMR, MS and X-ray diffraction is provided.