The present work highlights the facile and substantially streamlined microwave assisted synthesis of chalcones 3(a–m) from acetylpyrazolone 1 a and aldehyde 2(a–m) in piperidine‐ethanolic medium. The organocatalytic action of piperidine has been proposed in a mechanism. Different physical and analytical methods have been used to characterize the synthesized chalcones. Single Crystal XRD analyses of compounds 3 e and 3 f also supported proposed interpretation of the structural arrangements of these molecules. Further the synthesized compounds were evaluated for DPPH activity and results were compared with standard quercetin. Following compounds; 3 h, 3 i, 3 j and 3 d articulated excellent antioxidant activity.