This study describes synthesis and characterization of new liquid crystal aldoximes and aldoxime ethers in detail. Firstly, 4′-(6-bromohexyloxy)biphenyl-4-carbonitrile, 4′-(8-bromooctylox)biphenyl-4-carbonitrile and 4′-(10-bromoodecyloxy)biphenyl-4-carbonitrile derivatives were synthesized, respectively. Then, with this compound, condensation reaction was determined to p-hydroxybenzaldehyde and new aldehyde derivatives were synthesized. This aldehyde derivatives were converted to new oxime derivatives, not found in the literature. Then, these new oxime derivatives were converted to oxime ether derivatives with iodomethane. All of the obtained products were characterized by a combination of FT-IR, 1H NMR, 13C NMR and elemental analysis. Then, the liquid crystal properties of these new compounds were determined by using DSC and POM techniques.