Abstract The cholestanol (5α-cholestan-3β-ol) esters of amino acids were synthesized with an interest for their possible biochemical activities. The cholestanol esters of glycine, l-alanine, β-alanine, l-leucine and l-aspartic acid were synthesized by a direct fusion of the two components under the passing of hydrogen chloride through the reactants. That of glutamic acid was prepared by using quinoline hydrochloride as a solvent. From the condensation product of aspartic acid and cholestanol, mono- and di-ester were isolated. The monocholestanol ester of aspartic acid was also synthesized by the Gabriel process.