MoSe2 layers, synthesized by annealing a molybdenum foil under selenium pressure, have been investigated by scanning electron microscopy, X-ray analysis, electron spectroscopy (XPS) and electrical resistance measurements. It has been found that stoichiometric layers are obtained after appropriate processing. The films crystallize in the hexagonal structure. The crystallites develop preferentially along the c axis. The binding energies deduced from the XPS lines were found to be in good agreement with those of the reference powder. The electrical resistance is governed by hopping conduction in the low temperature range (80–250 K) and by grain boundary scattering mechanisms at higher temperatures.