The microwave assisted synthesis of diethyl 2,3‐diaryltetrahydro‐4,5‐isoxazoledicarboxylates by the cycloaddition of diethyl maleate with appropriate nitrones was carried out. The conformational aspects of the title compounds were investigated by NMR and X‐ray studies and the features are compared with a set of related tetrahydroisoxazoles highlighting the effect of substituents on the conformation of central five mem‐bered ring.