An e cient synthesis of 4,4 0-(phenylmethylene)bis(1H-pyrazol-5-ol)-3carboxylates is achieved by one-pot pseudo ve-component reaction of phenylhydrazine, acetylenedicarboxylates, and aromatic aldehydes in the presence of nano-NiZr4(PO4)6 at 60 C in water. Nano-NiZr 4 (PO 4) 6 has been characterized by powder X-Ray Di raction (XRD) and Scanning Electronic Microscopy (SEM). Use of simple and readily available starting materials, excellent yields in short time, reusability of the catalyst, little catalyst loading, and simple operational procedures are some of the important features of this protocol.