Efficient One‐Pot Four‐Component Synthesis and X‐ray Crystallographic Structure of 2‐Pyridone Derivatives

A series of 3‐cyano‐2‐pyridone derivatives were synthesized by one‐pot four‐component condensation reaction involving a benzaldehyde derivative, alkyl cyanoacetate, acyclic or cyclic ketones, and ammonium acetate in reflux condition. The X‐ray structure of the products 5a and 5d confirm symmetric dimers via hydrogen bonding interactions between individual pyridine molecules showing, in addition, also π–π stacking interactions.     

Efficient Method for Oxidation of Ketones to Esters with 4-Aminoperoxybenzoic Acid Supported On Silica Gel

4-Aminoperoxybenzoic acid supported on silica gel was found to be a versatile and efficient oxidant for the oxidation of ketones to esters.     

Taguchi OA16 orthogonal array design for the optimization of cloud point extraction for selenium determination in environmental and biological samples by tungsten-modified tube electrothermal atomic absorption spectrometry

Orthogonal array design (OAD) was applied for the first time to optimize cloud point extraction (CPE) conditions for Se(IV) determination by electrothermal atomic absorption spectrometry (ETAAS) in environmental and biological samples. Selenium was reacted with o-phenylenediamine to form piazselenol in an acidic medium (pH 2). Using Triton X-114, as surfactant, piazselenol was quantitatively extracted into small volume (about 30 μL) of the surfactant-rich phase after centrifugation. Five relevant factors, i.e. surfactant concentration, pH, ionic strength, equilibrium time and temperature were selected and the effects of each factor were studied at four levels on the extraction efficiency of Se(IV) and optimized. The statistical analysis revealed that the most important factors contributing to the extraction efficiency are ionic strength, pH and percent of surfactant. Based on the results obtained from the analysis of variance (ANOVA), the optimum conditions for extraction were established as: pH 6; vial temperature = 50 °C; extraction time = 7 min and 0.3% (w/v) of Triton X-114. The method was permitted to obtain a detection limit of 0.09 ng mL⁻¹ and two linear calibration ranges from 0.6 to 1.0 and 1.0 to 80.0 ng mL⁻¹ Se. The precision (%RSD) of the extraction and determination for the six replicates of Se at 20 ng mL⁻¹ was better than 3.6% and the enrichment factor of 63.5 was achieved. The studied analyte was successfully extracted and determined with high efficiency using cloud point extraction method in water and biological matrices.     

PTSA catalyzed simple and green synthesis of benzothiazole derivatives in water

Abstract  

p-Toluenesulfonic acid (10 mol%) was found to be an effective and efficient catalyst for the synthesis of 2-substituted benzothiazoles from aromatic aldehydes and 2-aminothiophenol in moderate to excellent yields in water. This method provides a simple and efficient protocol in terms of mild reaction conditions, clean reaction profiles, small quantity of catalyst, and simple workup procedure.     

Developments in hollow fiber based liquid-phase microextraction: principles and applications

Hollow fiber liquid-phase microextraction (HF-LPME) offers an efficient alternative to classical techniques for sample preparation and preconcentration. Features include high selectivity, good enrichment factors, and improved possibilities for automation. HP-LPME relies on the extraction of target analytes from aqueous samples into a supported liquid membrane (SLM) sustained in the pores of the wall of a porous hollow fiber, and then into an acceptor phase (that can be aqueous or organic) in the lumen of the hollow fiber. After extraction, the acceptor solution is directly subjected to a chemical analysis. HP-LPME can be performed in either the 2- or 3-phases mode. In the 2-phase mode, the organic solvent is present both in the porous wall and inside the lumen of the hollow fiber. In the 3-phase mode, the acceptor phase can be aqueous and this results in a conventional 3-phase system compatible with HPLC or capillary electrophoresis. Alternatively, the acceptor solution is organic and this represents a 3-phase extraction system with two immiscible organic solvents that is compatible with all common analytical instruments. In HP-LPME methods based on the use of SLMs, the mass transfer occurs by passive diffusion, and high extraction yields as well as efficient extraction kinetics are obtained by applying a pH gradient. In addition, active transport can be performed by using carrier or applying an electrical potential across the SLM. Due to high analyte preconcentration, excellent sample clean-up, and low consumption of organic solvent, HF-LPME has a large application potential in areas such as drug analysis and environmental monitoring. This review focuses on the fundamentals of extraction principles, technical implementations, and future trends in HF-LPME.

Simultaneous spectrophotometric determination of uranium and zirconium using cloud point extraction and multivariate methods

A cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to simultaneous extraction and spectrophotometric determination of uranium and zirconium from aqueous solution using partial least squares (PLS) regression is investigated. The method is based on the complexation reaction of these cations with Alizarin Red S (ARS) and subsequent micelle-mediated extraction of products. The chemical parameters affecting the separation phase and detection process were studied and optimized. Under the optimum experimental conditions (i.e. pH 5.2, Triton X-114?=?0.20%, equilibrium time 10?min and cloud point 45?°C), calibration graphs were linear in the range of 0.01?C3?mg?L^?1 with detection limits of 2.0 and 0.80???g L^?1 for U and Zr, respectively. The experimental calibration set was composed of 16 sample solutions using an orthogonal design for two component mixtures. The root mean square error of predictions (RMSEPs) for U and Zr were 0.0907 and 0.1117, respectively. The interference effect of some anions and cations was also tested. The method was applied to the simultaneous determination of U and Zr in water samples.     

Novel coated-graphite membrane sensor based on N,N′-dimethylcyanodiaza-18-crown-6 for the determination of ultra-trace amounts of lead

A novel selective membrane electrode for determination of ultra-trace amount of lead was prepared. The PVC membrane containing N,N′-dimethylcyanodiaza-18-cown-6 (DMCDA18C6) directly coated on a graphite electrode, exhibits a Nernstian response for Pb²⁺ ions over a very wide concentration range (from 1.0×10⁻² to 1.0×10⁻⁷ M) with a limit of detection of 7.0×10⁻⁸ M (∼14.5 ppb). It has a fast response time of ∼10 s and can be used for at least 2 months without any major deviation in potential. The electrode revealed very good selectivity with respect to all common alkali, alkaline earth, transition and heavy metal ions. The proposed sensor was used as an indicator electrode in potentiometric titration of lead ions and in determination of lead in edible oil, human hair and water samples. The proposed sensor was found to be superior to the best Pb²⁺-selective electrodes reported in terms of detection limit and selectivity coefficient.     

Synthesis of MnAl2O4 nanocrystallites by Pechini and sequential homogenous precipitation methods: characterization, product comparison, photocatalytic effect, and Taguchi optimization

Nanocrystalline manganese aluminate (MnAl₂O₄) has been synthesized by Pechini and sequential homogenous precipitation methods and the results have been compared. The Taguchi L₄ statistical design was utilized to optimize the production of MnAl₂O₄ nanoparticles by Pechini method. The MnAl₂O₄ nanocrystallites obtained by Pechini and sequential homogenous precipitation methods had the average particle size of 26.5 and 49.5 nm, respectively. The products were characterized with X-ray diffraction, laser light scattering, thermogravimetry analysis, Fourier transform infrared, UV–visible, energy dispersive X-ray, scanning electron microscope and inductively coupled plasma analyses. The photocatalytic activities of MnAl₂O₄ nanoparticles synthesized by two methods were investigated using aqueous solution of methylene blue under irradiation of visible light.