Synthesis,Characterization, and Biological Evaluation of 10H‐Phenothiazines,Their Sulfones and Ribofuranosides

10H‐phenothiazines are synthesized via Smiles rearrangement. These prepared phenothiazines act as a base to prepare ribofuranosides by treating them with b‐D ‐ribofuranosyl‐1‐acetate‐2,3,5‐tribenzoate. 10H‐phenothiazines on refluxing with hydrogen peroxide in glacial acetic acid gave 10H‐phenothiazine‐5,5‐dioxides. The synthesized compounds were evaluated for their antioxidative properties through in vitro studies, and they are also screened for their antimicrobial activity. The structure of the synthesized compounds has been established by elemental analysis and spectroscopic data.     

Microwave-assisted synthesis of 1,3-dialkyl ethers of calix[4]arenes: application to the synthesis of cesium selective calix[4]crown-6 ionophores

Partial etherification of phenolic-OH groups of calix[4]arenes with various alkyl halides/tosylates and K₂CO₃ under microwave irradiation afforded 1,3-dialkoxycalix[4]arenes in their cone conformation only as predominant/sole product in good yields (71–85%). The protocol was found to be much superior to conventional heating both in terms of yield and reaction time. Some of the 1,3-dialkoxycalix[4]arenes were elaborated further to the syntheses of cesium selective calix[4]crown-6 ionophores.     

Cyclomicrobuxine monohydrate

In the title compound, 3β‐(dimethylamino)‐16α‐hydroxy‐14‐methyl‐4‐methylene‐9,19‐cyclo‐5α‐pregnan‐20‐one monohydrate, C₂₅H₃₉NO₂·H₂O, the pentacyclo steroidal alkaloid is composed of three six‐membered, one five‐membered and one three‐membered ring. The molecular dimensions are as expected. The structure is stabilized by hydrogen bonds involving H and O atoms of water and the alkaloid molecules, with strong N?O [2.829 (7) Å] and O?O [2.790 (6) and 2.949 (7) Å] interactions.     

rac-BINAP-PdCl2 catalyzed Heck reactions of 3-formylquinolin-2-yl chlorides with methyl acrylate: synthesis of methyl 3-(3-formylquinolin-2-yl) acrylates

rac-BINAP-PdCl₂ catalytic system catalyzed Heck reaction of 3-formylquinolin-2-yl chlorides with methyl acrylate in DMA is described to the synthesis of methyl 3-(3-formyl-quinolin-2-yl)-acrylates, in good to excellent yields. The reaction could be also extended with other activated alkenes to afford Heck products. Fused-benzene ring in heterocyclic and carbocyclic moieties was found to enhance the yields.     

A visual strip sensor for determination of iron

A visual strip has been developed for sensing iron in different aqueous samples like natural water and fruit juices. The sensor has been synthesized by UV-radiation induced graft polymerization of acrylamide monomer in microporous poly(propylene) base. For physical immobilization of iron selective reagent, the in situ polymerization of acrylamide has been carried out in the presence of 1,10-phenanthroline. The loaded strip on interaction with Fe(II) in aqueous solution turned into orange red color and the intensity of the color was found to be directly proportional to the amount of Fe(II) in the aqueous sample. The minimal sensor response with naked eye was found for 50 ng mL⁻¹ of Fe in 15 min of interaction. However, as low as 20 ng mL⁻¹ Fe could be quantified using a spectrophotometer. The detection limit calculated using the 3s/S criteria, where ‘s’ is the standard deviation of the absorbance of blank reagent loaded strip and ‘S’ is the slope of the linear calibration plot, was 1.0 ng mL⁻¹. The strip was applied to measure Fe in a variety of samples such as ground water and fruit juices.     

Three‐dimensional structure of cyclic antibiotic teicoplanin aglycone using NMR distance and dihedral angle restraints in a DMSO solvation model

The three‐dimensional solution conformation of teicoplanin aglycone was determined using NMR spectroscopy. A combination of NOE and dihedral angle restraints in a DMSO solvation model was used to calculate an ensemble of structures having a root mean square deviation of 0.17 Å. The structures were generated using systematic searches of conformational space for optimal satisfaction of distance and dihedral angle restraints. Comparison of the NMR‐derived structure of teicoplanin aglycone with the X‐ray structure of a teicoplanin aglycone analog revealed a common backbone conformation with deviation of two aromatic side chain substituents. Experimentally determined backbone ¹³C chemical shifts showed good agreement with those computed at the density functional level of theory, providing a cross validation of the backbone conformation. The flexible portion of the molecule was consistent with the region that changes conformation to accommodate protein binding. The results showed that a hydrogen‐bonded DMSO molecule in combination with NMR‐derived restraints together enabled calculation of structures that satisfied experimental data. Copyright © 2015 John Wiley & Sons, Ltd.     

Glass transition and crystallization kinetics analysis of Sb–Se–Ge chalcogenide glasses

Differential thermal analysis (DTA) has been employed to investigate the effect of Ge addition on the glass transition behavior and crystallization kinetics of Sb₁₀Se_90?xGe_x (x = 0, 19, 21, 23, 25, 27) alloys. The three characteristic temperatures viz. glass transition (T _g), crystallization (T _c), and melting (T _m) have been determined and found to vary with the heating rates and Ge content. Thermal stability and glass forming tendency have been evaluated in terms of ΔT (= T _c ? T _g) and reduced glass transition temperature. The activation energies for glass transition and crystallization have been used to analyze the nucleation and growth process. The activation energy analysis also determines the suitability of alloys to be used in switching applications. Results have been interpreted in terms of bond energies and structural transformations in the investigated alloys.     

Nanocrystalline Zn1−x Ag x O y thin films evolved through electrodeposition for photoelectrochemical splitting of water

Nanocrystalline Zn_1???x Ag _x O _y (x?=?10^??3???50?×?10^??3) thin films evolved through electrodeposition over ITO substrate have been investigated for photoelectrochemical splitting of water. Samples were characterized by XRD, EDX, SEM, AFM, UV–visible optical absorption, and Mössbauer spectral analysis. Ag incorporation led to a decrease in the band gap energy and alterations in microstructural and semiconductor properties. Raising Ag concentration in samples up to 1 % at. caused a significant reduction in density and electrical resistivity, enhanced absorption along with red shift to the band gap energy, anodic shift in flat band potential, and increased charge carrier density, enabling 1 % at. Ag-incorporated ZnO films most photosensitive by yielding highest short-circuit current, photocurrent density, and applied bias photon to current efficiency. Plausible reasons have been offered.     

Electroanalytical Studies of Chromone Based Ionophores for the Selective Determination of Arsenite Ion

Two chemosensors 4H‐1‐benzopyran‐3‐carboxaldehyde, 4‐oxo‐, 3‐(2‐phenylhydrazone), [I₁] and 4H‐1‐benzopyran‐3‐carboxaldehyde, 4‐oxo‐, 3‐[2‐(2,4‐dinitrophenyl)hydrazone], [I₂] with hydrazone‐NH group as binding site have been shown excellent selectivity for arsenite ion. It is confirmed by the UV‐vis titration that I₂ is more selective than I₁. The performance of the coated graphite electrode (CGE) was found to be better than polymeric membrane electrode (PME) in terms of linear range of 4.89×10^?7–1.0×10^?1 mol L^?1, low detection limit of 8.31×10^?8 mol L^?1 and short response time. The proposed sensors were also used to determine the arsenite ion in different water samples.