Finely dispersed palladium on silk‐fibroin as an efficient and ligand‐free catalyst for Heck cross‐coupling reaction

A palladium–fibroin complex (Pd/Fib.) was prepared by the addition of sonicated fibroin fiber in water to palladium acetate solution. Pd (OAc)₂ was absorbed by fibroin and reduced with NaBH₄ at room temperature to the Pd(0) nanoparticles. Powder‐X‐ray diffraction, scanning electron microscopy–energy‐dispersive X‐ray spectroscopy, Fourier transform‐infrared, CHN elemental analysis and inductively coupled plasma‐atomic emission spectroscopy were carried out to characterize the Pd/Fib. catalyst. Catalytic activity of this finely dispersed palladium was examined in the Heck coupling reaction. The catalytic coupling of aryl halides (‐Cl, ‐Br, ‐I) and olefins led to the formation of the corresponding coupled products in moderate to high yields under air atmosphere. A variety of substrates, including electron‐rich and electron‐poor aryl halides, were converted smoothly to the targeted products in simple procedure. Heterogeneous supported Pd catalyst can be recycled and reused several times.     

Preparation of an efficient catalyst through injection of CuI on modified poly (styrene-co-maleic anhydride) and theoretical investigation of the structural and electronic properties of catalyst

A novel polymer supported [poly (styrene-co-maleic imide) (SMI)]Cu(I) nano-particles was prepared via in situ reaction of 4-amino-5-methyl-4H-1,2,4-triazole-3-thione with [poly (styrene-co-maleic anhydride)] (SMA) along with immobilization of CuI. These nano-particles were fully characterized by using scanning electron microscopy (SEM), energy dispersive spectroscopy analysis, Xray (EDAX), inductively coupled plasma (ICP) analysis, ¹H NMR and FT-IR techniques. Moreover, the structural and electronic features of metal–ligand interactions in the complex model of polymer-supported copper nanocatalyst were assessed using density functional theory calculations. The catalytic activity of these supported Cu(I) nonoparticles was examined in one of the classiest name reaction so–called “click reaction” which is coined K. B Sharpless for the regioselective synthesis of 1,2,3-triazole derivatives using a multicomponent reaction (MCR) involving benzyl halides, sodium azide and terminal alkynes in water as a green solvent. This heterogeneous catalyst showed excellent catalytic activity and was separated by simple filtration and was used at least in five consecutive runs without a significant decrease in its activity.     

Preyssler heteropolyacid supported on silica coated NiFe2O4 nanoparticles for the catalytic synthesis of bis(dihydropyrimidinone)benzene and 3,4-dihydropyrimidin-2(1H)-ones

A novel magnetic acidic catalyst comprising Preyssler (H14[NaP5W30O110]) heteropoly acid support‐ed on silica coated nickel ferrite nanoparticles (NiFe2O4@SiO2) was prepared. The catalyst was character...     

An Eco‐friendly Three Component Manifold for the Synthesis of α‐Aminophosphonates under Catalyst and Solvent‐free Conditions,X‐ray Characterization and Their Evaluation as Anticancer Agents

A series of α‐aminophosphonates were synthesized through one‐pot condensation of aryl aldehydes, aryl amines and diethyl phosphite in the absence of any catalyst and organic solvents. All the synthesized α‐aminophosphonates were characterized by spectral and elemental analysis and in the case of compound 4j by X‐ray crystallography. Some of these new α‐aminophosphonate derivatives were found to have cytotoxic activity on the cancer cell line DU145 in vitro by the MTT method.     

A microextraction procedure based on a task‐specific ionic liquid for the separation and preconcentration of lead ions from red lipstick and pine leaves

First, the extraction and preconcentration of ultratrace amounts of lead(II) ions was performed using microliter volumes of a task‐specific ionic liquid. The remarkable properties of ionic liquids were added to the advantages of microextraction procedure. The ionic liquid used was trioctylmethylammonium thiosalicylate, which formed a lead thiolate complex due to the chelating effect of the ortho‐positioned carboxylate relative to thiol functionality. So, trioctylmethylammonium thiosalicylate played the roles of both chelating agent and extraction solvent simultaneously. Hence, there is no need to use a ligand. The main parameters affecting the efficiency of the method were investigated and optimized. Under optimized conditions, this approach showed a linear range of 2.0–24.0 ng/mL with a detection limit of 0.0010 ng/mL. The proposed method was applied to the extraction and preconcentration of lead from red lipstick and pine leaves samples prior to electrothermal atomic absorption spectroscopic determination.     

Ag3[PMo12O40]: An efficient and green catalyst for the synthesis of highly functionalized pyran‐annulated heterocycles via multicomponent reaction

A facile, efficient and eco‐friendly catalytic protocol was developed for the synthesis of medicinally important pyran‐annulated heterocycles via multicomponent reaction (MCR). Cyclocondensation of differently substituted aromatic aldehydes, malononitrile/ethyl cyanoacetate and various β‐dicarbonyl compounds in the presence of Ag₃[PMo₁₂O₄₀]?nH₂O as heterogeneous catalyst, in EtOH–H₂O, afforded diverse pyran‐fused chromene analogues. The merits observed for this approach were it being conducted via MCR, using commercially available or easily accessible starting materials in the presence of a green and easily separable heterogeneous and reusable catalyst, and affording high yields of desired products in very short reaction times with high purity in one‐pot fashion, thus providing a superior alternative approach for the synthesis of pyran‐annulated heterocycles.