The Heck reaction (HR) generates a carbon–carbon bond by coupling aromatic or vinyl halide with a terminal alkene. A Pd catalyst, amine base, and organic solvent are used in this reaction. Mild conditions such asaqueous solutions, mild bases, and room temperature are also maintained. HR prepares biologically active organic compounds, heterocyclic compounds, nanomaterials, mimics of natural products, drugs, and other complex compounds with many biological applications. Zinc aluminate, ZnAl2O4, a spinel-structured ternary oxide with thermochemical stability, reduced surface acidity, considerable mechanical strength, low sintering temperature, wide band gap, and excellent optical properties, has garnered attention as an advanced material in recent years. Thus, it is employed as a high-temperature material, sensor, electronic, optical, and also as a catalytic support material. This study performed the Heck reaction, O-allylation, and C-allylation without palladium catalyst, amine as base, or other solvents. This protocol used microwave irradiation (MWR)and nano-sized zinc aluminate (ZnAl2O4) as a base, solid support, and catalyst. Thus, this reaction methodology is a greener oneand maintainsatom economy-. To achieve affordable and clean energy, we developed one of the most unequivocal methodologies for sequential coupling and cyclization to produce only 8-membered oxa-aza heterocycles by MWRwithout any extraneous base. To our knowledge, this is the first study of nano-sized ZnAl2O4 catalysed chemical synthesis of benzoxocinoquinolines using HR.