Selective Silylation of Alcohols,Phenols and Oximes Using N‐Chlorosaccharin as an Efficient Catalyst under Mild and Solvent‐Free Conditions

Efficient silylation of OH group in alcohols, phenols and oximes is described using a catalytic amount of N‐chlorosaccharin and hexamethyldisilazane (HMDS) under mild and solvent‐free conditions. This silylation reaction can be carried out with excellent and interesting various selectivities.     

Application of a new fiber coating based on electrochemically reduced graphene oxide for the cold‐fiber headspace solid‐phase microextraction of tricyclic antidepressants

A new fiber based on the electrochemical reduction of graphene oxide was prepared on a copper wire for solid‐phase microextraction (SPME) applications. The prepared fiber was used for the SPME and gas chromatographic analysis of tricyclic antidepressants (TCADs), including amitriptyline, trimipramine, and clomipramine. The feasibility of direct‐immersion and headspace modes of SPME for the determination of TCADs was studied. The effects of four parameters including pH, salt content, extraction temperature with and without cooling the fiber, and extraction time were investigated. The comparison showed that headspace cold fiber SPME results in the best outcome for the extraction of TCADs. Under the optimized conditions of this mode, the calibration curves were linear between 2.0 and 500 ng/mL and the detection limits were between 0.30 and 0.53 ng/mL. The intraday and interday RSDs obtained at 20 ng/mL (n = 5), using a single fiber, were 5.5–9.0 and 7.5–9.8, respectively. The fiber to fiber repeatability (n = 4), expressed as the RSD, was between 12.8 and 13.2% at a 20 ng/mL concentration level. The method was successfully applied to the analysis of TCADs in plasma samples showing recoveries from 73 to 96%.     

Thermosensitive molecularly imprinted poly(1‐vinyl‐2‐pyrrolidone/methyl methacrylate/N‐vinylcaprolactam) for selective extraction of imatinib mesylate in human biological fluid

The efficiency of a molecularly imprinted polymer as a selective packing material for the solid‐phase extraction of imatinib mesylate sorption was investigated. The molecularly imprinted polymer was prepared using N,N′‐methylenebisacrylamide as a cross‐linker agent, N‐vinylcaprolactam as a thermo‐sensitive monomer, 1‐vinyl‐2‐pyrrolidone and methyl methacrylate as functional monomers, azobisisobutyronitrile as an initiator and imatinib mesylate as a template. The drug‐imprinted polymer was identified by Fourier transform infrared spectroscopy, thermogravimetric analysis, elemental analysis, and scanning electron microscopy. It was found that this polymer can be used for determination of trace levels of imatinib mesylate with a recovery percentage that could reach over 90%. Furthermore, the synthesized molecularly imprinted polymer indicated higher selectivity towards imatinib mesylate than other compounds. From isotherm study, the equilibrium adsorption data of imatinib mesylate by imprinted polymer were analyzed by Langmuir, Freundlich, and Temkin isotherm models. The developed method was used for determination of imatinib mesylate in human fluid samples by high performance liquid chromatography with excellent results.     

Synthesis of julolidines via one-pot cascade three component Povarov reaction in the presence of silica sulfuric acid

In this report, synthesis of julolidines via one-pot cascade reaction of aniline derivatives with a mixture of styrene and formaldehyde in the presence of silica sulfuric acid as an efficient catalyst has been studied under aerobic condition. By presented method, various julolidines are obtained under mild and transition metal-free conditions. The reaction is proceeded with imine formation and followed by an Aza-Diels-Alder cycloaddition with styrene gave julolidine derivatives. The catalyst can be recycled and reused multiple times to catalyze the reaction.     

Ultrasound-promoted solvent-free aza-Michael addition of p-toluenesulfonamide to fumaric esters by potassium carbonate: Synthesis of p-toluenesulfonamide derivatives

An efficient, mild, inexpensive and eco-friendly protocol for the synthesis of p-toluenesulfonamide derivatives by aza-Michael addition reaction of p-toluenesulfonamide to fumaric esters using potassium carbonate under ultrasound irradiation was developed. This method is simple, convenient and the desired compounds are produced in good to excellent yield. The bulkiness of alkoxy group (–OR) of fumaric esters did not affect significantly on the yields and reaction times. This reaction worked well on linear and nonlinear alkyl fumarates. The reaction, surprisingly, was not successful on methyl fumarate. In this case methyl fumarate has been hydrolyzed to fumaric acid under reaction conditions.     

Synthesis and Characterization of Co3O4 Nanoparticles by Thermal Treatment Process

The simple preparation of Co₃O₄ nanoparticles from a solid metallorganic molecular precursor [bis(salicylaldehydeato)cobal(II)]; [Co(sal)₂] has been achieved via two simple steps: firstly, the [Co(sal)₂] precursor was precipitated from the reaction of cobalt(II) acetate and salicylaldehyde; in propanol under nitrogen condition; then, cubic phase Co₃O₄ nanoparticles with the size of mostly 20–30 nm could be produced by thermal treatment of the [Co(sal)₂] in air at 500 °C for 5 h. The as-synthesized products were characterized by powder XRD, FT-IR, TEM and SEM. The results confirm that the resulting oxide was pure single-crystalline Co₃O₄ nanoparticles. The optical absorption spectrum indicates that the direct band gaps of Co₃O₄ nanoparticles are 1.53 and 2.02 eV. The optical property test indicates that the absorption peak of the nanoparticles shifts towards short wavelength, and the blue shift phenomenon might be ascribed to the quantum effect. The hysteresis loops of the obtained samples reveal the ferromagnetic behaviors the enhanced coercivity (H _c ) and decreased saturation magnetization (M _s ) in contrast to their respective bulk materials.     

Holographic dark energy in Brans–Dicke theory with logarithmic correction

In the derivation of holographic dark energy density, the area law of the black hole entropy plays a crucial role. However, the entropy-area relation can be modified from the inclusion of quantum effects, motivated from the loop quantum gravity, string theory and black hole physics. In this paper, we study cosmological implication of the interacting entropy-corrected holographic dark energy model in the framework of Brans–Dicke cosmology. We obtain the equation of state and the deceleration parameters of the entropy-corrected holographic dark energy in a non-flat Universe. As system’s IR cutoff we choose the radius of the event horizon measured on the sphere of the horizon, defined as L = ar(t). We find out that when the entropy-corrected holographic dark energy is combined with the Brans–Dicke field, the transition from normal state where w _D > −1 to the phantom regime where w _D < −1 for the equation of state of interacting dark energy can be more easily achieved for than when resort to the Einstein field equations is made.