Combustion Derived Nanocrystalline‐ZrO2 and Its Catalytic Activity for Biginelli Condensation under Microwave Irradiation

Nanocrystalline zirconium(IV) oxide (nc‐ZrO₂) possessing high surface area was synthesized by a low temperature eco‐friendly solution combustion method using a new organic fuel alanine. The powder XRD, SEM and surface area measurements were carried out for characterization of nc‐ZrO₂. The powder XRD results revealed that, the nc‐ZrO₂ has the pure tetragonal phase. The crystallite size calculated by Scherrer's formula and BET surface area were found to be ca. 53–57 nm and ca. 275 m²/g, respectively. SEM micrograph exhibited the macroporous nature of the powder. nc‐ZrO₂ has been employed as a catalyst for the solvent‐free synthesis of 3,4‐dihydro‐ pyrimidin‐2‐ones (DHPMs) by a microwave (MW) assisted one‐pot, multicomponent Biginelli condensation reaction of araldehydes, ethylacetoacetate and urea or thiourea. DHPMs are obtained in good to excellent yields (85%–96%) under this reaction condition within short interval of time (10–20 min).     

One-pot approach for the synthesis of 2-aryl benzothiazoles via a two-component coupling of gem-dibromomethylarenes and o-aminothiophenols

One-pot synthesis of 2-aryl benzothiazoles from gem-dibromomethylarenes using 2-aminoarylthiols is described. Benzothiazoles were obtained in high chemical yields under mild conditions. This transformation would facilitate synthesis by short reaction times, large-scale synthesis, easy and quick isolation of the products, which are the main advantages of this procedure.     

PCC-Promoted Dehydration of Aldoximes: A Convenient Access to Aromatic,Heteroaromatic, and Aliphatic Nitriles

A simple and convenient procedure for the synthesis of nitriles by dehydration of aldoximes using a PCC (pyridiniumchlorochromate) has been developed. A variety of aromatic, heteroaromatic, and aliphatic aldoximes are converted.

Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the full spectral details.     

A hybrid electrochemical–thermal method for the preparation of large ZnO nanoparticles

A simple and efficient two-step hybrid electrochemical–thermal route was developed for the synthesis of large quantity of ZnO nanoparticles using aqueous sodium bicarbonate electrolyte and sacrificial Zn anode and cathode in an undivided cell under galvanostatic mode at room temperature. The bath concentration and current density were varied from 30 to 120 mmol and 0.05 to 1.5 A/dm². The electrochemically generated precursor was calcined for an hour at different range of temperature from 140 to 600 °C. The calcined samples were characterized by XRD, SEM/EDX, TEM, TG-DTA, FT-IR, and UV–Vis spectral methods. Rietveld refinement of X-ray data indicates that the calcined compound exhibits hexagonal (Wurtzite) structure with space group of P63mc (No. 186). The crystallite sizes were in the range of 22–75 nm based on Debye–Scherrer equation. The TEM results reveal that the particle sizes were in the order of 30–40 nm. The blue shift was noticed in UV–Vis absorption spectra, the band gaps were found to be 5.40–5.11 eV. Scanning electron micrographs suggest that all the samples were randomly oriented granular morphology.     

Synthesis and Crystal Structure Studies of Novel Bioactive Heterocycle: 7-Chloro-5-Cyclopropyl-9-Methyl-10-(2-Piperidin-1-yl-Ethyl)-5,10-Dihydro-4,5,6,10-Tetraaza-Dibenzo[a,d] Cyclohepten-11-One

Abstract  The compound, 7-chloro-5-cyclopropyl-9-methyl-10-(2-piperidin-1-yl-ethyl)-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one, C₂₂H₂₆N₅ClO, crystallizes in the triclinic space group Pī with cell parameters a = 8.918(7) ?, b = 9.297(7) ?, c = 14.184(8) ?, V = 1095.98(1) ?³ and Z = 2. The final residual factor R ₁ = 0.0451. The structure exhibits intermolecular hydrogen bonds. The 2-piperidin-1-yl-ethyl ring adopts a chair conformation. The starting material used to synthesize the title compound is the intermediate compound of well known anti-HIV drug Nevirapine hence the title compound is having biological importance and hence this crystal structure will helps to structural characterization of the molecule and also for the molecular modeling it will helps for biological study. Graphical Abstract  The title compound 7-chloro-5-cyclopropyl-9-methyl-10-(2-piperidin-1-yl-ethyl)-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one was synthesized by condensation of 7-chloro-5-cyclopropyl-9-methyl-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one with 1-(2-chloro-ethyl)-piperidine hydrochloride in presence of anhydrous powdered potassium carbonate as base using N,N-dimethyl formamide as solvent and its crystal structure determined. The title compound derived from bioactive molecule and it is also having biological importance hence this crystal structure will helps for the structural characterization and the biological study of the novel molecule.      

Formation of crystalline Na2V6O16·3H2O ribbons into belts and rings

Single-crystalline nanobelts and nanorings of Na(2)V(6)O(16)·3H(2)O structures have been facilely synthesized through a direct hydrothermal reaction between NaVO(3) and H(3)PO(4), without the addition of any harmful solvents or surfactants. The analytical techniques of scanning electron microscopy, transmission electron microscopy (TEM), powder X-ray diffraction, thermogravimetric analysis, energy-dispersive X-ray spectroscopy, Fourier transform infrared, high-resolution TEM, and selected-area electron diffraction have been used to characterize the morphology, composition, and structure of the synthesized products. The Na(2)V(6)O(16)·3H(2)O nanobelts are up to several hundreds of micrometers in length and 100-300 nm in thickness, and for nanorings, the diameters are 4.5-6.5 μm. H(3)PO(4) plays a key role in maintaining the pH of the solution as well as producing PO(4)(3-) ions in solution. The chemical reactions and a possible growth mechanism involved in the formation of Na(2)V(6)O(16)·3H(2)O nanobelts and nanorings are briefly discussed.     

Structural features of biologically active coordination compounds of vanillinsemicarbazone

Summary Complexes of vanillinsemicarbazone (VSC) with Mn^II, Fe^II, Co^II, Ni^II, Cu^II, Zn^II, Cd^II and Hg^II have been prepared and characterised by elemental analyses, molar conductance, magnetic susceptibility and spectral data. Probable structures for the complexes are suggested on the basis of their physico-chemical properties. The fungitoxicity of VSC and the isolated complexes have been tested on pathogenic fungi. On leave from the University of Mysore, India.     

Vanadium Oxide: From Gels to Nanotubes

Vanadium oxide nanotubes (VO _x -NT) have been prepared by mixing hexadecylamine with V₂O₅·nH₂O gels. This procedure was followed by an hydrothermal treatment (150–180°C, 2–7 days) which leads to a large quantity of VO _x -NT. SEM and XRD analysis have been used to optimize the temperature and reaction time required for production of VO _x -Nt and morphology of the nanotubes investigated by TEM.     

One-pot synthesis of benzimidazoles from gem-dibromomethylarenes using o-diaminoarenes

A one-pot synthesis of benzimidazoles from gem-dibromomethylarenes is described. The reaction shows the method to prepare a variety of benzimidazole analogues with excellent yield.