In this study, a novel and green heterogeneous catalyst KIT-6@SMTU@Ni was successfully synthesized via a new method of Ni(ii) complex stabilization on modified mesoporous KIT-6. The synthesized catalyst was characterized using various techniques. It was found to be efficient in the synthesis of 5-substituted 1H-tetrazoles and pyranopyrazoles, with high yields and reasonable reaction times. The catalyst also exhibited excellent reusability and had other advantages such as using green solvents and commercially available materials.
In this paper, KIT-6@SMTU@Ni was successfully synthesized via a new method of Ni(ii) complex stabilization on modified mesoporous KIT-6, as a novel and green heterogeneous catalyst. The obtained catalyst (KIT-6@SMTU@Ni) was characterized using Fourier transform infrared spectroscopy (FT-IR), Brunauer-Emmett-Teller (BET) calculation, X-ray diffraction (XRD), atomic absorption spectroscopy (AAS), energy-dispersive X-ray spectroscopy (EDS), X-ray mapping, thermogravimetric analysis (TGA) techniques and scanning electron microscopy (SEM). After complete characterization of the catalyst, it was successfully used for the synthesis of 5-substituted 1H-tetrazoles and pyranopyrazoles. Moreover, tetrazoles were synthesized from benzonitrile derivatives and sodium azide (NaN3). All tetrazole products were synthesized with high TON, TOF and excellent yields (88-98%) in a reasonable time (0.13-8 h), demonstrating the efficiency and practicality of the KIT-6@SMTU@Ni catalyst. Furthermore, pyranopyrazoles were prepared through the condensation reaction of benzaldehyde derivatives with malononitrile, hydrazine hydrate and ethyl acetoacetate with high TON, TOF and excellent yields (87-98%) at appropriate times (2-10.5 h). KIT-6@SMTU@Ni could be reused for five runs without any re-activation. Significantly, this plotted protocol has prominent benefits, such as applying green solvents, the use of commercially available and low-cost materials, excellent separation and reusability of the catalyst, short reaction time, high yield of products and a facile work-up.
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