Benzyl-substituted tin chalcogenides (Bn 3Sn) 2S (1) and (Bn 3Sn) 2Se (2) yield polycrystalline-phase pure SnS and SnSe in good ceramic yields when pyrolyzed with S and Se, respectively, at 275°C. Heating mixtures of (1) and elemental selenium produce solid solutions of the formula Sn(S xSe 1−x). Combustion analysis showed less than 1% residual carbon in all ceramic products. This methodology allows the complete conversion of tin to tin chalcogenides and eliminates the need to synthesize organosulfur and organoselenium intermediates.