Abstract: Pure 4-alkyl-1-phenylcyclohexanes (C_3, C_5, C_7) were prepared with acylation of cyclohexene, and their cis-trans-isomers were separated by chromatography. With new methods, two liquid crystals of 4-alkyl-1-(4-bromophenyl) cyclohexanes (C_3, C_5) and three new compounds of 4-alkyl-1-(4-iodophenyl) cyclohexanes (C_3, C_5, C_7) were synthesized with broruination and iodination. Three liquid crystals of 4-alkyl-1-(4-cyanophenyl) cyclohexanes (C_3, C_5, C_7) from iodizated compounds were also prepared. The structures of all the compounds prepared are proved to be correct by determination of element analysis, IR, MS and NMR. Transition temperatures of liquid crystal compounds prepared agree with what had already been reported before, and their yields are high. Reaction mechanism is also discussed.