Cyclohexylcarbamates of cellulose and amylose were prepared and their resolving abilities for enantiomers were evaluated as chiral stationary phases (CSPs) for high-performance liquid chromatography. The CSPs showed high resolving abilities, which are comparable to those of popular CSPs, tris(3,5-dmethylphenylcarbamate)s of cellulose and amylose. The cycloalkylcarbamates could also be used as CSPs for thin-layer chromatography because of the absence of a phenyl group, which causes the difficulty of detection by UV radiation. In addition, these two derivatives were soluble in chloroform and exhibited chiral discrimination to some chiral compounds in H-1 NMR spectroscopy as well as in HPLC.