In this work, twelve compounds: 5(+)-4-[(2-methylbutyloxycarbonyl)phenyl]4′-(4″-trans-n-alkylcyclohexyl)benzoates;S(+)-4-[(2-methylbutyloxy)phenyl]4′-(4″-trans-n-alkylcyclohexyl)benzoates, where alkyl = C5-C10, were synthesized. The effect of the alkyl chains on liquid crystal transition temperatures of two homologous series prepared has been investigated systematically. The mesomorphic properties are studied by DSC and Polarizing Microscopy. Chiral smectic C and chiral nematic mesophases, as well as a smectic A mesophase, in several cases, were observed.