In the present work, we studied the controlled growth of MoO3 nanostructures and their gas sensing performance. MoO3 NS were synthesized using thermal evaporation method. FE-SEM (LEO 1525) and XRD were used to characterize the morphology and crystallinity of MoO3 NS. Sensing devices were mounted on TO packages using electro-soldered gold wires, and they were tested toward some chemical compounds. These NS give reversible response to Acetone, Ethanol and H2 in a temperature range of 300–550 °C. MoO3 sensors exhibit a high response ∆G/G = 45 towards 50 ppm of Ethanol at 450 °C.