Tungsten-substituted molybdophosphoric acid impregnated with kaolin: effective catalysts for the synthesis of 3,4-dihydropyrimidin-2(1H)-ones via biginelli reaction.

A series of highly reusable heterogeneous catalysts (10-25 wt% PMo7W5/kaolin), consisting of tungsten-substituted molybdophosphoric acid, H3PMo7W5O40·24H2O (PMo7W5) impregnated with acid treated kaolin clay was synthesized by the wetness impregnation method. The newly synthesized catalyst was fully characterized using inductively coupled plasma-atomic emission spectroscopy (ICP-AES), Fourier transform infrared (FT-IR), powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) analysis and thermal analysis (TG-DTA). The synthesized materials were shown to be efficient in the synthesis of 3,4-dihydropyrimidin-2(1H)-ones via Biginelli reaction under solvent-free conditions. The obtained results indicate that 20% PMo7W5/kaolin catalyst showed remarkably enhanced catalytic activity compared to the bulk PMo7W5 catalyst, and also the (10 and 15%) PMo7W5 catalyst supported on kaolin clay.

Cesium salt of 2-molybdo-10-tungstophosphoric acid as an efficient and reusable catalyst for the synthesis of uracil derivatives via a green route.

A solid catalyst, cesium salt of 2-molybdo-10-tungstophosphoric acid (Cs2.3H0.7PW10Mo2O40) named as Cs-3, was synthesized by a simple, cheap, clean, and eco-friendly method. The physicochemical properties of the synthesized catalyst were studied via FTIR spectroscopy, XRD, EDX, ICP-AES, SEM-TEM, and BET techniques. The precursor 2-molybdo-10-tungstophosphoric acid (H3PW10Mo2O40) was easily soluble in water and other polar solvents. Moreover, their cesium salts Cs x H3-x PW10Mo2 with Cs content in the range x = 2.0-2.5 were insoluble in water and other polar solvents. The surface area of the precursor (5.483 m2 g-1) increased after partial proton exchange by Cs+ ions (111.732 m2 g-1), and all samples with x > 1 were resistant to leaching of active components and can be recycled without obvious loss of activity. This catalyst used for the synthesis of uracil derivatives via a green route under solvent free conditions at 70 °C gives higher yield within a shorter reaction time. The catalyst was found to be more active and reusable over nine runs with a negligible loss of activity.