The majority of organic ligands used to build porous coordination polymers feature a rigid, hydrocarbon-based central core that is substituted with coordinating functional groups (e.g., carboxylate) or have nitrogen heterocycles (imidazole, tetrazole, etc) as coordinating sites. Organic linkers having a heterocycle-based central unit have been underemployed for the generation of coordination polymers, and their use has been largely limited to commercially available compounds. This contribution aims at introducing three novel rigid, ditopic, carboxylate or hybrid ligands 1–3 having a pyrazole in the central core, useful for the preparation of porous coordination polymers.formulaThe reaction sequence leading to the desired ligands starts with the Claisen-like condensation between of diethyl oxalate with an acetophenone para-substituted either with cyano or with 4-(1H-imidazol-1-yl), followed by the reaction of the resulting 2,4-dioxobutanoate with phenylhydrazine. Next, simultaneous transformation of the nitrile and ester function in intermediate 4 under harsh hydrolysis conditions (KOH, water, reflux, 48 h) produces ligand 1, whereas ring closure of tetrazole leading to ligand 2 is performed by reacting the cyano group in intermediate 4 with NaN3. Ligand 3 is efficiently obtained through the mild hydrolysis (LiOH, THF–MeOH–water, rt, overnight) of the ester function in the corresponding imidazolesubstituted analogue of 4. The structures of the intermediates and the target compounds have been established by 1H- and 13C-NMR spectroscopy, and they are in agreement with the proposed structures. In addition, the structure of ligand 2 has been determined by single crystal X-ray diffraction experiments. Compound 2 crystallizes in space group P2(1)2(1)2(1) of orthorhombic system, with one neutral molecular unit of C17H12N6O2 in the asymmetric part, and unit cell parameters a = 5.8614(8) Å, b = 8.8381(10) Å, c = 28.489(4) Å.