New peroxovanadium compounds containing biogenic co-ligands: synthesis,stability and effect on alkaline phosphatase activity

A set of new diperoxovanadate(V) complexes with the dipeptides glycyl–glycine or glycyl–leucine as ancillary ligands of the type, A[VO(O₂)₂(peptide)(H₂O)] · H₂O, A = Na or K have been synthesized and characterized by elemental analysis, thermal analysis, magnetic susceptibility and spectral studies. The complexes contain side-on bound peroxo groups and a dipeptide zwitterion as co-ligand, binding the metal center unidentately through O (carboxylate) atom. The compounds are highly stable toward decomposition in solutions of acidic as well as physiological pH and serve as weak substrates to catalase, undergoing degradation in the presence of the enzyme at a rate much slower than H₂O₂. The compounds stoichiometrically oxidize GSH to GSSG. On comparing the GSH oxidizing ability of these compounds with those of previously reported peroxotungsten compounds containing similar co-ligands, a significant difference was noted. The compounds induce a strong inhibitory effect on alkaline phosphatase activity with a potency higher than that of the free peptides, vanadate, or peroxovanadate.     

Alga-mediated facile green synthesis of silver nanoparticles: Photophysical,catalytic and antibacterial activity

A facile, convenient and green method has been employed for the synthesis of silver nanoparticles (AgNPs) using dried biomass of a green alga, Chlorella ellipsoidea. The phytochemicals from the alga, as a mild and non-toxic source, are believed to serve as both reducing and stabilizing agents. The formation of silver nanoparticles was confirmed from the appearance of a surface plasmon resonance band at 436 nm and energy dispersive X-ray spectroscopy. The transmission electron microscopy images showed the nanoparticles to be nearly spherical in shape with different sizes. A dynamic light scattering study revealed the average particle size to be 220.8 ± 31.3 nm. Fourier transform infrared spectroscopy revealed the occurrence of alga-derived phytochemicals attached to the outer surface of biogenically accessed silver nanoparticles. The powder X-ray diffraction study revealed the face-centred cubic crystalline structure of the nanoparticles. The as-synthesized biomatrix-loaded AgNPs exhibited a high photocatalytic activity for the degradation of the hazardous pollutant dyes methylene blue and methyl orange. The catalytic efficiency was sustained even after three reduction cycles. A kinetic study indicated the degradation rates to be pseudo-first order with the degradation rate being 4.72 × 10⁻² min⁻¹ for methylene blue and 3.24 × 10⁻² min⁻¹ for methyl orange. The AgNPs also exhibited significant antibacterial activity against four selected pathogenic bacterial strains.     

The development of phosphinoamine–Pd(II)–imidazole complexes: implications in room‐temperature Suzuki–Miyaura cross‐coupling reaction

The reaction of N‐methylimidazole (N‐MeIm) and N‐butylimidazole (N‐BuIm) with the complexes [PdCl₂(PPh₂py–P,N)] and [PdCl₂(PPh₂Etpy–P,N)] in the presence of NH₄PF₆ under N₂ at room temperature afforded four new cationic Pd(II) complexes [PdCl(PPh₂py–P,N)(N‐MeIm)](PF₆) ( 1 ), [PdCl(PPh₂py–P,N)(N‐BuIm)](PF₆) ( 2 ), [PdCl(PPh₂Etpy–P,N)(N‐MeIm)](PF₆) ( 4 ) and [PdCl(PPh₂Etpy‐P,N)(N‐BuIm)](PF₆) ( 5 ) in good yields, where PPh₂py is 2‐(diphenylphosphino)pyridine and PPh₂Etpy is 2‐{2‐(diphenylphosphino)ethyl}pyridine). The complexes were fully characterized. The catalytic activities of these complexes were investigated for Suzuki–Miyaura cross‐coupling reactions at room temperature. Complex 2 exhibited excellent activity compared to other analogs. Copyright © 2013 John Wiley & Sons, Ltd.     

Highly efficient amine‐based catalytic system for room temperature Suzuki–Miyaura reactions of aryl halides with arylboronic acids

An in situ‐generated catalytic system based on PdCl₂ and primary amine‐based ligand exhibited excellent activity (up to 98% isolated yield) in the Suzuki–Miyaura cross‐coupling reactions of aryl bromides with arylboronic acids in water, at room temperature, without any additive. The efficiencies of the ligands follow the order: (C₆H₅)₃CNH₂ > C₆H₅CH₂ NH₂ > C₆H₅ NH₂ > C₆H₁₁ NH₂, which is in accordance with the palladacycle forming capacity of the respective ligands. Moderate‐to‐good yields (up to 78% isolated yield) of the coupling products were also obtained with less reactive aryl chlorides as substrates at room temperature in isopropanol using an alternative protocol based on Pd(OAc)₂ and (C₆H₅)₃CNH₂. Copyright © 2011 John Wiley & Sons, Ltd.     

Iron(0), rhodium(I) and palladium(II) complexes with p‐(N,N‐dimethylaminophenyl) diphenylphosphine and the application of the palladium complex as a catalyst for the Suzuki–Miyaura cross‐coupling reaction

The reaction of p‐(N,N‐dimethylaminophenyl)diphenylphosphine [PPh₂(p‐C₆H₄NMe₂)] with [Fe₃(CO)₁₂], [Rh(CO)₂Cl]₂ and PdCl₂ resulted in three new mononuclear complexes, {Fe(CO)₄[η¹‐(P)‐PPh₂(p‐C₆H₄NMe₂)]} ( 1a ), trans‐{Rh(CO)Cl[η¹‐(P)‐PPh₂(p‐C₆H₄NMe₂)]₂} ( 2 ) and trans‐{PdCl₂[η¹‐(P)‐PPh₂(p‐C₆H₄NMe₂)]₂} ( 3 ), respectively. A small amount of dinuclear nonmetal‐metal bonded complex, {Fe₂(CO)₈[µ‐(P,N)‐PPh₂(p‐C₆H₄NMe₂)]} ( 1b ), was also isolated as a side product in the reaction of [Fe₃(CO)₁₂]. The complexes were characterized by elemental analyses, mass, IR, UV–vis, ¹H, ¹³C (except 1b) and ³¹P{¹H} NMR spectroscopy. The Pd complex 3 effectively catalyzes the Suzuki–Miyaura cross‐coupling reactions of aryl halides with arylboronic acids in water–isopropanol (1:1) at room temperature. Excellent yields (up to 99% isolated yield) were achieved. The effects of different solvents, bases, catalyst quantities were also evaluated. Copyright © 2011 John Wiley & Sons, Ltd.     

Microwave-promoted efficient synthesis of spiroindenotetrahydropyridine derivatives via a catalyst- and solvent-free pseudo one-pot five-component tandem Knoevenagel/aza-Diels–Alder reaction

A microwave-assisted, one-pot pseudo five-component reaction strategy has been developed for the synthesis of some novel spiroindenotetrahydropyridine derivatives from 1,3-indanedione, an aromatic aldehyde, and ammonium acetate under catalyst- and solvent-free conditions via tandem Knoevenagel/aza-Diels–Alder reaction.     

Congruences for generalized Frobenius partitions with 4 colors

We present some congruences involving the functions c?₄(n) and which denote, respectively, the number of generalized Frobenius partitions of n with 4 colors and 4-order generalized Frobenius partitions of n with 4 colors.     

Preparation of cross-linked guar gum nanospheres containing tamoxifen citrate by single step emulsion in situ polymer cross-linking method

In the present work, guar gum nanospheres containing tamoxifen citrate (TC) were prepared and characterized for using it as a carrier for targeted drug delivery. Tamoxifen is a non steroidal drug used in the treatment of breast cancer. The compound administered to patients is the citrate salt of the trans isomer, tamoxifen citrate. Single step emulsion in situ polymer crosslinking technique was employed to prepare polymer coated drug nanoparticles. Model polymer used in this study was guar gum, which is commonly used for colon specific drug delivery in the pharmaceutical industry. During preparation four-different drug loading solvents were tried and dichloromethane provided the best drug loading result. Briefly, 5 mg drug was dissolved in dichloromethane and emulsified with an aqueous solution of guar gum using span 80 as emulsifier. Cross-linking was made by the use of cross linker glutaraldehyde during the process. A core shell type particles were observed. Drug load was confirmed by FT-IR and quantitated by HPLC. Nanoparticles were further characterized for particle size and morphology. Particle size between 200 and 300 nm were obtained. Influence of process variables on the size of nanoparticles were studied. It was observed that the concentration of polymer and stabilizer determined the size of nanoparticles.     

Optical properties of SnO2 nanoparticles

In recent times, considerable research efforts have been focused on the exploration of novel optical properties of nanocrystalline SnO₂ particles such as photoluminescence (PL). In the present work, spherical SnO₂ nanoparticles are synthesized by solid state reaction at different temperatures using tin chloride dihydrate and sodium hydroxide flakes as precursors. Transmission electron micrograph shows uniform and spherical SnO₂ nanoparticles of diameter 30–40 nm. Micro-Raman spectra show an inverse relationship of line-width with SnO₂ particle size. The band gap of SnO₂ is calculated by plotting (αhν)² vs. hν and extrapolating the linear portion of it to α = 0 and found it to be 3.76–4.24 eV. Photoluminescence intensity increases with the increase of solid state reaction temperature up to 873 K. This is attributed to the generation of the oxygen ion vacancies in SnO₂.