NiFe2O4 as a magnetically recoverable nanocatalyst for odourless C–S bond formation via the cleavage of C–O bond in the presence of S8 under mild and green conditions

We present green methodologies for one‐pot and odourless syntheses of unsymmetric and symmetric diaryl sulfides via C─O bond activation using NiFe₂O₄ magnetic nanoparticles as a reusable heterogeneous nanocatalyst. The synthesis of unsymmetric sulfides is performed using the cross‐coupling reaction of phenolic esters such as acetates, triflates and tosylates with arylboronic acid/S₈ or triphenyltin chloride/S₈ as thiolating agents in the presence of base and NiFe₂O₄ magnetic nanoparticles as a catalyst in poly(ethylene glycol) as solvent at 60–85°C. Also, the synthesis of symmetric diaryl sulfides from phenolic compounds using S₈ as the sulfur source and NiFe₂O₄ as catalyst in dimethylformamide at 120°C is described. Using these protocols, the syntheses of various unsymmetric and symmetric sulfides become easier than using the available protocols due to the use of a magnetically reusable bimetallic nanocatalyst and avoiding the use of thiols and aryl halides.     

Manganese(II), cobalts(II) and nickel(II) complexes of tris(2-pyridyl)phosphine and their catalytic activity toward oxidation of tetralin

Abstract  

Monomeric Mn²⁺, Co²⁺ and Ni²⁺ complexes of tris(2-pyridyl)phosphine (P(2-py)₃ were synthesized through the reaction of the hydrated metal(II) chlorides with P(2-py)₃ in near-quantitative yields. The solid-state structure of the Mn complex was determined by single-crystal X-ray diffraction. All three complexes were tested as homogeneous catalysts for the oxidation of tetralin to α-tetralone with tert-butyl hydroperoxide (TBHP) as oxidant. The influences of temperature, solvent, catalyst molar ratio and time of the reaction on the catalyzed reactions were investigated.     

Metallic impurities in graphenes prepared from graphite can dramatically influence their properties

All at C? Graphenes prepared by the top-down exfoliation of graphite are shown to contain metallic impurities (see scheme, metal impurities shown as black dots). These impurities may dominate their properties and can have a negative influence on their potential applications.     

Influence of chemical extraction conditions on the physicochemical and functional properties of polysaccharide gum from durian (Durio zibethinus) seed

Durian seed is an agricultural biomass waste of durian fruit. It can be a natural plant source of non-starch polysaccharide gum with potential functional properties. The main goal of the present study was to investigate the effect of chemical extraction variables (i.e., the decolouring time, soaking temperature and soaking time) on the physicochemical properties of durian seed gum. The physicochemical and functional properties of chemically-extracted durian seed gum were assessed by determining the particle size and distribution, solubility and the water- and oil-holding capacity (WHC and OHC). The present work revealed that the soaking time should be considered as the most critical extraction variable affecting the physicochemical properties of crude durian seed gum.     

Fluorescent imidazolium-based cyclophane for detection of guanosine-5'-triphosphate and I(-) in aqueous solution of physiological pH

A new water-soluble and fluorescent imidazolium-anthracene cyclophane (1) effectively recognizes the biologically important GTP and I(-) over other anions in a 100% aqueous solution of physiological pH 7.4. Fluorescence and (1)H NMR spectra and ab initio calculations demonstrate that emission arises from the formation of an excimer state and quenching occurs upon GTP/I(-) binding through (C-H)(+)···A(-) hydrogen bond interactions.     

An experimental investigation of substituent effects on the formation of 2,3‐dihydroquinazolin‐4(1H)‐ones: a kinetic study

The effect of different substituents on the kinetics of the reactions between 2‐amino‐benzamide and some of benzaldehyde derivatives have been spectrally investigated in the presence of formic acid. The proposed mechanism were challenged due to the determination of rate‐determining step (RDS) and also, to obtain the general rate law of the reaction. For all substituents, the reactions followed the second‐order kinetics and the partial orders of reactions were recognized with respect to each reactant. Electron withdrawing substituents on benzaldehyde ring increased the rate of reaction. Kinetic values (k and E_a) and associated activation parameters (ΔH^?, ΔG^? and ΔS^?) of the reactions were determined. Both the Arrhenius and the Eyring equations were used to calculate activation energy. Comparison of magnitude of and T showed that the reactions were enthalpy controlled. Isokinetic plots for the reactions were plotted and linear relationship between and recognized that relative contribution of enthalpy and entropy to the overall free energy was the same in the reactions.     

The influence of main emulsion components on the physicochemical properties of soursop beverage emulsions: A mixture design approach

The physicochemical properties of soursop beverage emulsion were investigated using mixture design. Results indicated that the regression models were significantly fitted for all response variables studied, except creaming index at 10°C. Interactions between biopolymers and oil phase had the most significant effect on creaming stability; however, modified starch played a much prominent role in maintaining the cloudiness and average droplet size. Meanwhile, WPI contributed significantly to the conductivity of the emulsions. The optimum condition resulted in desirable physicochemical properties could be achieved using 8.70% (w/w) modified starch, 1.02% (w/w) WPI, 10.11% (w/w) flavor oil, and 76.57% (w/w) water.     

A highly stable and efficient magnetically recoverable and reusable Pd nanocatalyst in aqueous media heterogeneously catalysed Suzuki C–C cross‐coupling reactions

Surface modification of Fe₃O₄ nanoparticles with triethoxyethylcyanide groups was used for the immobilization of palladium nanoparticles to produce Fe₃O₄/Ethyl‐CN/Pd. The catalyst was characterized using Fourier transform infrared, wavelength‐dispersive X‐ray, energy‐dispersive X‐ray and X‐ray photoelectron spectroscopies, field‐emission scanning electron and transmission electron microscopies, and X‐ray diffraction, vibrating sample magnetometry and inductively coupled plasma analyses. In this fabrication, cyano groups played an important role as a capping agent. The catalytic behaviour of Fe₃O₄/Ethyl‐CN/Pd nanoparticles was measured in the Suzuki cross‐coupling reaction of various aryl halides (Ar? I, Ar? Br, Ar? Cl) with phenylboronic acid in aqueous phase at room temperature. Interestingly, the novel catalyst could be recovered in a facile manner from the reaction mixture by applying an external magnet device and recycled seven times without any significant loss in activity. Copyright © 2015 John Wiley & Sons, Ltd.