Hydrothermal synthesis of a homologous series of thiophene derivatives from 4-(1-(hydroxyimino) ethyl) phenyl 4-alkoxybenzoates and thiophene-2-carboxylic acid using mercuric acetate under solvent-free conditions is described. The liquid crystalline properties of the synthesized compounds were investigated by Polarising Optical Microscopy (POM) and Differential Scanning Calorimetry (DSC). It is observed that all the members of the series exhibited only Nematic phase (N).