Two hybrid organic-inorganic materials, ZnS(1,3-diaminopropane) 1/2 {1} and ZnSe(m-xylylenediamine) 1/2 {2} were used as precursors of nanometric ZnS and ZnSe nanostructures. To obtain a single-phase semiconductor, refluxing in different solvents (acetonitrile, 1-octanol, 1,6-hexanediol) with various boiling points was applied. In this method, the synergic effect between temperature and the properties of the reactant medium was used to remove amines from hybrid material containing semiconducting slabs and to form pure nanometer-sized semiconducting grains whose properties were different than those of the corresponding bulk phases. The main goal of our research was to answer the question whether reaction conditions have an impact on the features of obtained semiconducting grains of ZnS and ZnSe. Accordingly, all obtained samples were analyzed using the powder diffraction method, UV-vis spectroscopy and scanning electron microscopy.