Polymeric catalyst for the synthesis of new pyrido[2,3-b]indoles

A new and efficient method has been developed for the one-pot synthesis of novel 2,9-dihydro-2-oxo-4-aryl-1H-pyrido[2,3-b]indole-3-carbonitrile derivatives by condensation of substituted (triethoxymethyl)arene, 1-methyl-1H-indol-2-ol and cyanoacetamide in the presence of a catalytic amount of crosslinked poly(2-acrylamido-2-methyl propane sulfonic acid) (AMPS) as an efficient and heterogeneous catalyst. This polymeric solid acid catalyst is stable and can be easily recovered and reused without significant change in its activity.     

Mechanistic insight into the hydrogenation of acetylene on the Pd2/g-C3N4 catalyst: effect of Pd clustering on the barrier energy and selectivity

Structural Chemistry - In this work, the hydrogenation of acetylene on the Pd2/g-C3N4 catalyst is investigated by the density functional theory (DFT) and quantum theory of atoms in molecules...     

Synthesis of chromene derivatives in the presence of mordenite zeolite/MIL‐101 (Cr) metal–organic framework composite as catalyst

In the present study, the synthesis of mordenite zeolite/MIL‐101(Cr) metal–organic framework (MOF) composite [MOR/MIL‐101(Cr)] using the ship in a bottle method was suggested. The properties of prepared composite and individual MOF and MOR zeolite were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption–desorption measurement, and thermogravimetric analysis (TGA). The XRD results indicated diffraction peaks for each compound (MOR and MOF) in composite. The SEM and TEM images showed the formation of plates MOR (with size of 2.5 × 3 μm) along with spherical particles MIL‐101. The Brunauer–Emmett–Teller results showed that the surface area of the composite was smaller than individual MOF and MOR zeolite. Based on TGA plots, the hybrid zeolite/MOF composite was more thermally stable compared with the isolated MIL‐101(Cr). The composite was functionalized by post‐synthetic modification to obtain acid–base bifunctionality (H‐MOR/MIL‐101‐ED) for the synthesis of chromene derivatives. The acidity from framework Al‐O(H)‐Si sites in MOR and basicity from amine groups in MIL‐101 were obtained by post‐synthetic modification.     

Synergetic catalytic effect of rGO,Pd, Fe3O4 and PPy as a magnetically separable and recyclable nanocomposite for coupling reactions in green media

In this paper, rGO/Pd–Fe₃O₄@PPy as an efficient stable nanocomposite was synthesized. To understand the synergetic effects of rGO, Pd, Fe₃O₄ and PolyPyrrole, the performance of rGO/Pd–Fe₃O₄@PPy as a heterogeneous recyclable nanocatalyst in the green synthesis of C‐C and C‐O coupling products, as well as different conditions are studied. Synthesized rGO/Pd–Fe₃O₄@PPy was characterized by FT‐IR, XRD, FE‐SEM, EDS, TGA and AFM analysis. Best results are obtained under sonication in H₂O for C‐C coupling and by ball‐milling for C‐O coupling. The benefits of this method include: green solvents and conditions, absence of external base, low reaction times with high yield and easy work‐up method.     

Application of a dispersive micro‐solid‐phase extraction method for pre‐concentration and ultra‐trace determination of cadmium ions in water and biological samples

A method for the trace determination of cadmium ions in water, human urine and human blood serum samples using ultrasonic‐assisted dispersive micro‐solid‐phase extraction (UA‐D‐μSPE) was developed. Silica‐coated magnetic nanoparticles were coated with polythiophene, and the resulting sorbent was characterized using thermogravimetry, differential thermal analysis, scanning electron microscopy, Fourier transform infrared spectrometry and X‐ray diffraction. Following UA‐D‐μSPE, cadmium ions were quantified using graphite furnace atomic absorption spectrometry. A Box–Behnken design was used for optimization of important sorption and desorption parameters in UA‐D‐μSPE: in the sorption step, pH of solution, sorption amount and sonication time for sorption; in the desorption step, concentration of eluent, volume of eluent and sonication time. The optimum conditions for the method were: pH of solution, 7.5; sonication time for sorption, 3 min; sorption amount, 35 mg; type and concentration of eluent, HCl and 1.1 mol l^?1; volume of eluent, 360 μl; sonication time for desorption, 110 s. Under the optimized conditions the limit of detection and relative standard deviation for the detection of cadmium ions by UA‐D‐μSPE were found to be 0.8 ng l^?1 and <6%, respectively.     

Preparation of bismuth sulfide nanoparticles as targeted biocompatible nano-radiosensitizer and carrier of methotrexate

In this study, Bi₂S₃@BSA–Bio–MTX nanoparticles (NPs) were synthesized for the first time by bovine serum albumin (BSA)-mediated biomineralization (Bi₂S₃@BSA NPs) followed by covalent bonding of biotin (Bio) and methotrexate (MTX) on the surface of the Bi₂S₃@BSA NPs via carbodiimide chemistry. The synthesized NPs were globular and exhibited uniform morphology with a hydrodynamic diameter of 107.6 ± 6.81 nm (mean ± standard deviation) and zeta potential of −20.9 ± 2.18 mV. Drug release from Bi₂S₃@BSA–Bio–MTX NPs indicated an enzyme-dependent release pattern. The in vitro biocompatibility of NPs was confirmed by investigating their cytotoxicity against the HEK-293 cell line and hemolysis assay test, whereas the in vivo biocompatibility of the NPs was evaluated and confirmed by the lethal dose 50 (LD₅₀) test. To evaluate the in vitro anticancer activity of the functionalized NPs and MTX, their cytotoxic effects was assessed against 4T1 cancer cells by 5-dimethylthiazol-z-yl)-2,5-diphenyltetrazolium bromide (MTT) assay with and without X-ray radiation. Results showed that Bi₂S₃@BSA–Bio–MTX NPs have excellent anticancer activity, especially following X-ray radiation.     

Pd(0)-guanidine@MCM-41: a very effective catalyst for rapid production of bis (pyrazolyl)methanes

In this research, a rapid, green and efficient protocol for synthesis of bis (pyrazolyl)methane derivatives in the presence of Pd(0)-guanidine@MCM-41 catalysts under solvent-free conditions by the following two methods has been reported: (i) via the one-pot pseudo five-component reaction among phenylhydrazine (2 equivalents), ethyl acetoacetate (2 equivalents) and aromatic aldehydes (1 equivalent); and (ii) the one-pot pseudo three-component reaction between 3-methyl-1-phenyl-1H-pyrazol-5(4H)-one (2 equivalents) and aromatic aldehydes (1 equivalent). Some advantages of this protocol include: green conditions, extremely short times, high efficiency, proper one-pot operation, generality of method, easy work-up and recyclability, and reusability of the catalyst up to five times without significant loss in catalytic activity.     

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.