Recently, methodologies that are in accordance with green chemistry principles have been garnering increasing attention. One of the most applied methods in this field is heterogeneous catalysis. In this context, many catalysts have been developed, and there is one remarkable class that has emerged: hybrid materials. Such heterogeneous catalysts are developed from organic and inorganic portions, especially from amino acids and metal salts, which are commonly found in the literature. Herein, we introduce Zn[Pro](2) and Zn[Gly](2) as heterogeneous catalysts in thio-Michael reactions via the implementation of two methods: via (1) a magnetic stirrer and (2) via an ultrasound device; the latter method resulted in minimally increased reaction yields in all cases.