Highly crystalline Cu9S5 (Cu1.8S), CuSe, PbS, and PbSe are obtained by reacting the elements in 2-mercaptoethanol as the solvent for 24 h at room temperature. The elemental reactions of copper and lead with sulfur in ethylene glycol were successful, yielding CuS and PbS, respectively. Metal sulfide formation was not observed using dimercaptoethane.