Nanoscale Mg(OH2) and MgO is prepared via a polyol-mediated synthesis. With concern to the experimental conditions, spherical particles, 20 and 100 nm in size are realized. Dynamic light scattering proves the presence of non-agglomerated and monodispersed Mg(OH)(2) in as-prepared suspensions of diethylene glycol. Based on the results of infrared spectroscopy, thermal analysis and X-ray powder diffraction, as-prepared Mg(OH)(2) can be dehydrated at a surprisingly low temperature (300 degrees C) to form MgO with almost similar particle size and shape.