Transition metal chalcogenides (TMC) is a broad class of materials comprising binary, ternary, quaternary, and multinary oxides, sulfides, selenides, and tellurides. These materials have application in different areas such as solar cells, photocatalysis, sensors, photoinduced therapy, and fluorescent labeling. Due to the technological importance of this class of material, it is necessary to find synthetic methods to produce them through procedures aligned with the Green Chemistry. In this sense, this chapter presents opportunities to make the solution chemistry synthesis of TMC greener. In addition to synthesis, the chapter presents different techniques of experimental planning and analysis, such as design of experiments, life cycle assessment, and machine learning. Then, it explains how Green Chemistry can benefit from each one of these techniques, and how they are related to the Green Chemistry Principles. Focus is placed on binary chalcogenides (sulfides, selenides, and tellurides), and the quaternary sulfide Cu2ZnSnS4 (CZTS), due to its application in many fields like solar energy, photocatalysis, and water splitting. The Green Chemistry synthesis, characterization, and application of these materials may represent sustainable and effective ways to save energy and resources without compromising the quality of the produced material.