Li2CoPO4F has been synthesized via a novel two-step reaction from a solvothermally prepared precursor mixture of LiCoPO4 and LiF. Solvent influences were monitored by powder X-ray diffraction and the reaction conditions for the conversion, of the precursor mixture to Li2CoPO4F were optimized. In addition, the obtained materials were characterized before and after carbon-coating by SEM, N-2 sorption, elemental and thermogravimetric analysis. The electrochemical performance of the products as high-voltage cathode materials in a coin-cell was tested, and long term stability over 50 charge/discharge cycles could be demonstrated. (C) The Author(s) 2015. Published by ECS. All rights reserved.