Hydrogenation of 4-cholesten-3-one (1) with tritium gas over palladium black in pyridine afforded [beta-4,5-H-3]-cholestan-3-one (2a). Tritium NMR showed that there was a mixture of tritiated compounds formed, 2a-2c; the latter two containing small amounts of protium substitution. Tritium NMR also indicated that none of the unwanted alpha-diastereomer was formed.