Synthesis of Arylidene – Isoquinolinones bearing Combretastatin Skeleton by Cyclocarbopalladation/cross coupling Tandem Heck-Suzuki Miaura Reactions using nano catalyst Pd@Py-IL-SPION

Cyclocarbopalladation/cross-coupling cascade intramolecular Heck–Suzuki–Miyaura reactions is applied for the first time by palladium immobilized on pyridine-imidazolium ionic liquid supported magnetic iron oxide nanoparticle catalyst (denoted Pd@Py-IL-SPION) for the last step to synthesize trisubstituted arylidene–isoquinolinones derivatives having Combretastatin skeleton. The reaction is performed via propargylamide intermediates prepared by Ugi 4-CR reactions, which undergoes intramolecular Heck–Suzuki–Miyaura domino reaction to produce the desired trisubstituted arylidene-isoquinolinones. The method shows full regio- and stereoselectivity derives from the particular Pd-catalyzed syn-insertion of triple bond.     

Synthesis,Hirshfeld surface analysis,luminescence and thermal properties of three first-row transition metal complexes containing 4′-hydroxy-2,2′:6′,2″-terpyridine: Application for preparation of nano metal oxides

A series of new mono- and bis-terpyridine complexes [Mn(tpyOH)Cl₂] ( 1 ), [Ni(tpyOH)₂](PF₆)₂ ( 2 ) and [Zn(tpyO)(η¹-OCOCH₃)(H₂O)]⋅3H₂O ( 4 ) containing 4′-hydroxy-2,2′:6′,2″-terpyridine (tpyOH) were synthesized and structurally characterized using elemental analysis, infrared spectroscopy and single-crystal X-ray diffraction. The reaction of MnCl₂ with tpyOH in a mixture of methanol and CH₂Cl₂ resulted in the formation of 1 . The X-ray crystal structure of 1 reveals that Mn(II) is penta-coordinated by three nitrogen atoms from tpyOH and two Cl⁻ in a slightly distorted trigonal bipyramidal geometry. Complex 2 was also prepared by the reaction of nickel(II) chloride with tpyOH in a methanolic medium in the presence of NH₄PF₆. Notably, the complex [Ni(tpyOH)(tpyO)]PF₆ ( 3 ), obtained during the crystallization of 2 from dichloromethane, was characterized using X-ray crystallography which shows that six nitrogen atoms from terpyridine ligands occupy the coordination sites around the Ni(II) centre in a distorted octahedral geometry with four longer bonds and two shorter Ni N bonds. The reaction of zinc(II) acetate with tpyOH in a mixture of methanol and CH₂Cl₂ led to the formation of 4 . The crystal structure of 4 reveals the formation of penta-coordinated Zn(II) complex containing three nitrogen atoms from tpyO, a monodentate acetate ligand and one coordinated water molecule. Hirshfeld surface analyses and two-dimensional fingerprint plots show that the main interactions are O…H/H…O contacts in 1 , 3 and 4 . The thermal decomposition reactions of 1 , 2 and 4 were studied using thermogravimetric analysis in detail due to their different structures. The solution luminescence features of 1 , 2 and 4 include high-energy intense π → π* intraligand and low-energy metal-to-ligand charge transfer transitions at room temperature. The calcination of the coordination complexes led to the formation of corresponding nano metal oxides. The products were structurally characterized using infrared spectroscopy, scanning electron microscopy and energy-dispersive X-ray spectroscopy. The average particle size using Scherrer's equation was calculated to be below 50 nm.     

Retracted: A new class of copper(I) complexes with imine-containing chelators which show potent anticancer activity

Seven novel complexes (C₁–C₇) were synthesized by the interaction between Cu(I) metal cation, L₁, L₂, L₃, X and PPh₃, where L₁–L₃ are derivatives of ((pyridine-2-ylmethylene)amino)phenol imine ligands and X = Cl⁻, Br⁻, I⁻, NCS⁻. All the complexes were characterized using infrared, ¹H NMR and ³¹P NMR spectroscopies. The crystal structures of C₁–C₇ were also determined using single-crystal X-ray diffraction. The organization of the crystal structures and the intermolecular interactions are discussed. The supramolecular assemblies are driven by cooperative π…π interactions and hydrogen bonds, followed by CH…π linkages. The potential anticancer effect of C₁–C₇ was assessed for human glioblastoma cells using several anticancer experiments, which showed that these complexes have marked anticancer property against U87 cells. It was also found that the minimum and maximum anticancer effects are shown by C₃- and C₄-treated samples, respectively. Furthermore, theoretical approaches were used to investigate the nature of metal–ligand interactions which suggest a closed-shell and electrostatic character for Cu…N, Cu…P and Cu…X bonds.     

Tuning Human Serum Albumin (HSA) Hydrogels through Albumin Glycation

The changes of technological properties of albumin-based hydrogels induced by increasing degrees of post-translational modification of the protein are reported. Maillard-type modification of amino acids arginine and lysine of albumin is achieved through glyoxal as an α-dicarbonyl compound. The degrees of modification are fine-tuned using different molar ratios of glyoxal. Hydrogels are thermally induced by heating highly concentrated precursor solutions above the protein's denaturation temperature. While the post-translational modifications are determined and quantified with mass spectrometry, continuous-wave (CW) electron paramagnetic resonance (EPR) spectroscopy shed light on the protein fatty acid binding capacity and changes thereof in solution and in the gel state. The viscoelastic behavior is characterized as a measure of the physical strength of the hydrogels. On the nanoscopic level, the modified albumins in low concentration solution reveal lower binding capacities with increasing degrees of modification. On the contrary, in the gel state, the binding capacity remains constant at all degrees of modifications. This indicates that the loss of fatty acid binding capacity for individual albumin molecules is partially compensated by new binding sites in the gel state, potentially formed by modified amino acids. Such, albumin glycation offers a fine-tuning method of technological and nanoscopic properties of these gels.     

Green and mild laccase-catalyzed aerobic oxidative coupling of benzenediol derivatives with various sodium benzenesulfinates

The oxidative coupling reaction between hydroquinone or catechols and various sodium benzenesulfinates was investigated using the laccase from Trametes versicolor, in the presence of O₂ in a phosphate buffer solution at room temperature to afford sulfonyl benzenediols in 75–95% yield.     

Preparation and Characterization of Functionalized Polyaniline-Based Nanocomposite as an Antibacterial Agent

Polyaniline-co-phenylenediamine (PAn/PDA) nanocomposite has been prepared in the aqueous medium using sodium dodecyl benzene sulfonate (DBSNa) and hydroxypropylcellulose (HPC) as a surfactant. The tests used in this research to characterize the products were SEM, TEM, FTIR, UV–Visible and TGA for morphology, particle size, chemical structure and stability. The results confirm that the spherical nanocomposites (40–90 nm) were formed with high thermal stability. It is shown in the results that the physicochemical properties of poly(alkyl substituted anilines) are depended on the substituent groups that are bonded to N-position. The prepared nanocomposites were then tested for the antibacterial properties against three pathogenic strains. The antibacterial properties of nanocomposites were investigated by disk diffusion, minimum inhibitory concentration (MIC), minimum bactericidal concentrations (MBC), and bactericidal kinetic methods. The disk diffusion result indicated that the diameter of the inhibition zones of PAn/PDA–HPC nanocomposite was 9, 11, and 10 mm against E. coli, P. aeruginosa, and S. aureus respectively. It was found that the value of MIC of PAn/PDA–HPC nanocomposite against E. coli, P. aeruginosa and S. aureus were 2.5, 1.25 and 2.5 mg/mL respectively. The evaluation results revealed the PAn/PDA–HPC nanocomposite exhibited excellent inhibitory activity against both gram-negative and gram-positive bacteria.     

Synthesis and characterization of aryl substituted functionalized graphene sheets and their electrochemical behavior

Journal of Solid State Electrochemistry - We report the electrochemical behavior of free-standing functionalized graphene sheet electrode in a potential window corresponding to that of high-voltage...