Synthesis and Characterization of Silica@Copper Core–Shell Nanoparticles: Application for Conjugate Addition Reactions

Silica@copper (SiO₂@Cu) core–shell nanoparticles were synthesized and well characterized by XRD, TEM, AFM, XPS, UV/Vis, TGA–MS, and ICP–AES techniques. The synthesized SiO₂@Cu core–shell nanoparticles were employed as catalysts for the conjugate addition of amines to α,β‐unsaturated compounds in water to obtain β‐amino carbonyl compounds in excellent yields in shorter reaction times. Furthermore, the catalyst works well for hetero‐Michael addition reactions of heteroatom nucleophiles such as thiols to α,β‐unsaturated compounds. As the reaction is performed in water, it allows for easy recycling of the catalyst with consistent activity.     

Friedel-Crafts alkylation of indoles with epoxides catalyzed by nanocrystalline titanium(IV) oxide

Friedel-Crafts alkylation of indoles with epoxides to afford 3-alkyl indole derivatives at room temperature with moderate to good yields and high regioselectivity using nanocrystalline titanium(IV) oxide catalyst is described.     

Operational characteristics and power scaling of a transverse flow transversely excited CW CO<Subscript>2</Subscript> laser

Transverse flow transversely excited (TFTE) CO₂ lasers are easily scalable to multikilowatt level. The laser power can be scaled up by increasing the volumetric gas flow and discharge volume. It was observed in a TFTE CW CO₂ laser having single row of pins as an anode and tubular cathode that the laser power was not increasing when the discharge volume and the gas volumetric flow were increased by increasing the electrode separation keeping the gas flow velocity constant. The discharge voltage too remained almost constant with the change of electrode separation at the same gas flow velocity. This necessitated revision of the scaling laws for designing this type of high power CO₂ laser. Experimental results of laser performance for different electrode separations are discussed and the modifications in the scaling laws are presented.     

Quasi-intramolecular acid–base reactions in aqueous solutions of metal-complexes of basic ligands I. Generalized theoretical considerations on the deammoniation of [ML m ]X n type ammonia complexes

The theoretical investigation on the distribution of chemical species obtainable as a function of the temperature of the aqueous solutions of metal complexes containing a basic ligand, altogether with the solubility relationship of the compounds to be formed, offers a simple means of planning the preparation of various types of complexes, double and single salts of the central metal cation and onium type compounds of protonated ligand of the central ion and the anion.     

Polarographic determination of deltamethrin

The electrochemical characteristics of deltamethrin have been determined by means of electrochemical techniques such as d.c. polarography, cyclic voltammetry and differential pulse polarography over a wide range of pH from 2.0-12.0. The title compound exhibits a single well defined peak due to the reduction of the CC moiety present in deltamethrin. The overall reduction process is diffusion-controlled and adsorption free in nature. The variation of half-wave potential with the pH, concentration of the title compound, and other experimental conditions is described. A possible mechanism for the reduction is suggested. The number of electrons involved in the electrode reduction is two. Investigation was also undertaken for the determination of deltamethrin in vegetables and in storage bags of rice and wheat under FCI's storage system.     

Characterization and reactivity of copper oxide catalysts supported on TiO2-ZrO2

A series of copper catalysts supported on TiO2-ZrO2 with copper loading varying from 1.0 to 21.6 wt % were prepared by a wet impregnation method. The catalysts were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy, electron spin resonance (ESR), temperature programmed reduction (TPR), and Brunauer-Emmett-Teller specific surface area measurements. Copper dispersion and metal area were determined by N2O decomposition by the passivation method. XRD results suggest that the copper oxide is present in a highly dispersed amorphous state at copper loadings <16.8 wt % in the sample and as a crystalline CuO phase at higher Cu loadings. Copper dispersion increases with Cu loading up to 5.1 wt % and levels off at higher loadings. The XPS peak intensity ratios of Cu 2p(3/2)/Ti 2p(3/2) and Cu 2p(3/2)/Zr 3d(5/2) were compared with the copper dispersion calculated from N2O decomposition. ESR results suggest the presence of two types of copper species on the TiO2-ZrO2 support. TPR profiles reveal the presence of highly dispersed copper oxide at lower temperatures and bulk CuO at higher temperatures. The catalytic properties were evaluated for the vapor-phase dehydrogenation of cyclohexanol to cyclohexanone and related to the dispersion of Cu on TiO2-ZrO2.     

Bromine Complexes of Polyvinylpyrrolidone Supports: A Mild Reagent for the Transformation of α‐Oxoketene Dithioacetals to β‐Oxothiolesters

When α‐oxoketene dithioacetals 1a–n were treated with the bromine complex of a copolymer of 1‐vinyl‐2‐pyrrolidone and 4‐vinylpyridine, the corresponding thiolcarboxylates 2a–n were formed in excellent yields. The reaction also works with other 1‐vinyl‐2‐pyrrolidone‐derived polymers as well as commercially available polyvinylpyrrolidone–bromine complexes. The method is suitable for preparing aliphatic, aromatic, and γ,δ‐unsaturated β‐oxothiolcarboxylates.     

Sonochemical Synthesis of 1,4‐Disubstituted 1,2,3‐Triazoles in Aqueous Medium

An ultrasound‐accelerated fast and efficient three‐component reaction for the regioselective synthesis of l,4‐disubstituted 1,2,3‐triazoles using different alkyl and allyl halides, terminal alkynes, and sodium azide in water at room temperature has been developed using CuI as catalyst. Ultrasonication dramatically decreases the reaction times.     

A simultaneous TG-DTG-DSC-quadrupole mass spectrometric study

Mechanistic aspects of the thermal decomposition of benzyl-triethyl-ammonium tetrafluoroborate (BTEATFB) employing simultaneous TG-DSC coupled with a quadrupole mass spectrometer are considered in this work. The experiments were conducted in an inert atmosphere of helium. The decomposition of BTEATFB proceeds through several competing mechanisms. While nucleophilic substitution reaction occurs through the formation of a tertiary amine and plays an important role in the initial stages of the decomposition, and the probability of Hoffman elimination also exists.