Layered oxides Li2MoO3 were synthesized at 923 K (sample A), 1023 K (sample B), and 1073 K (sample C) and characterized by X-ray diffractometry, magnetic and electrochemical measurements. All Li2MoO3 showed rhombohedral symmetry with an alpha-NaFeO2-related structure and paramagnetic behavior down to 83 K. Lithium. deintercalation from samples B and C proceeded to x=1.2 in Li2-xMoO3. The Li/Li2MoO3 (samples B and C) cells showed cycling capacities of 150 mAh/g in the voltage range of 1.5-4.3 V after 10 cycles. Samples B and C showed better cycle reversibility than sample A. The different charge and discharge characteristics between samples A-C might be caused by structural differences which were indicated by X-ray diffraction measurements.