A novel, lamellar type Vanadium n-propylamino phosphate catalyst is synthesized and characterized by using various physicochemical techniques such as Powder X-ray diffraction, Scanning electron microscopy/Energy dispersive X-ray analysis, Thermogravimetry/Differential thermal analysis, Fourier transform Infrared analysis, Electron spin resonance spectroscopy, Ultraviolet -Visible Diffuse reflectance spectroscopy, X-ray Photoelectron spectroscopy, 31 P Magic angle spinning Nuclear Magnetic Resonance spectroscopy and Catalytic applications toward Octahydroquinazolinone synthesis. It is found that the n-propylamine is present as sandwich between Vanadyl phosphate layers. Most of the Vanadium is present as V 4+ ions in tetrahedral co-ordination. Vanadium n-propylamino phosphate catalyses Octahydroquinazolinone synthesis more effeciently and the optimum conditions required for Octahydroquinazolinone synthesis are, Benzaldehyde (2 mmol), Dimedone (2 mmol), Urea (4 mmol), Methanol + Water (1:1, 5 mL) and Catalyst (0.05 g). A plausible mechanism is also proposed.
A novel vanadium dodecylamino phosphate was synthesised by an instant reaction between phosphoric acid and vanadyl acetylacetonoate using dodecylamine as the structure-directing agent at ambient temperature. The physicochemical characteristics of the material were investigated by a variety of analytical techniques. XRD studies revealed the presence of vanadium phosphate and hydrated vanadium phosphate phases in the framework of the material. The catalytic application of this material toward in the synthesis of polyhydroquinolines via Hantzsch condensation was investigated at ambient temperature. This method affords high yields within short reaction times. The influence of various reaction parameters such as different solvents, catalyst dosage, effect of aldehydes, and reusability was studied and a plausible mechanism proposed.
Novel titanium containing solid core mesoporous shell silica has been synthesized by using octadecyltrichloro silane and triethylamine. The synthesized material was characterized by various physicochemical techniques. The mesoporous character of the material has been revealed from PXRD studies. The presence of octadecyltrichloro silane and triethylamine in the sample has been confirmed from EDAX studies. TG/DTA analysis reveals the thermal characteristics of the synthesized material. The presence of titanium in the frame work and its coordination state has been studies by UV-vis DR studies and XPS analysis. Chemical environment of Si in the framework of the material has been studied by
29SiMASNMR studies. The surface area of the material is found to be around 550 m 2 g −1 and pore radius is of nano range from BET analysis. The spherical morphology and particle size of the core as well as shell has been found to be 300 nm and 50 nm respectively from TEM analysis. The catalytic application of this material towards the synthesis of caprolactam from cyclohexanone in presence of hydrogen peroxide through ammoxidation reaction has been investigated. The optimum conditions for the reaction have been established. The plausible mechanism for the formation of core silica and conversion of cyclohexanone has been proposed.
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