Iodine-Catalyzed Addition of Methyl Thioglycolate to Chalcones

Abstract

A series of novel β-mercapto carbonyl compounds (3a–z), methyl 2-(3-oxo-1,3-diarylpropylthio)acetate, were synthesized and characterized via iodine-catalyzed addition of methyl thioglycolate to chalcones (1a–z).

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Synthesis of melamine based polymer complexes and their thermal degradations and magnetic properties

In this study, new polymer Fe(III) and Cr(III) complexes were synthesized. These polymer complexes were characterized by using elemental analysis, FT-IR spectroscopy, MS, thermal analyses and magnetic susceptibility measurement technics. Their thermal degradations were investigated, and co-polymerization was compared to aliphatic polymerization by using 1,2-dibromomethylbenzene and o-phenylenedialdehyde. Finally, metal ratios of the complexes were determined by using atomic absorption spectroscopy. The complexes are distorted octahedral low-spin (S = 1/2) Fe(III) and distorted octahedral (S = 3/2) Cr(III) bridged by COO^? and catechol groups.     

Sensitive,Accurate and Selective Determination of Cd(II) Using Anodic Stripping Voltammetry with in-situ Hg-Bi Film Modified Pencil Graphite Electrode After Magnetic Dispersive Solid Phase Microextraction

This paper describes a novel approach to detect Cd(II) using the combination of the differential pulse anodic stripping voltammetry and magnetic nanoparticle based dispersive solid phase microextraction as an efficient, green and accurate method. Currents of Cd(II) increased linearly in the range from 75 to 2000 ng L⁻¹ Cd(II) with a detection limit of 21.6 ng L⁻¹. The RSD values of 2.6 and 6.0 % for 1.00 and 0.10 μg L⁻¹ respectively showed that proposed method has an acceptable repeatability. Recovery values between 92.3 and 98.6 % showed that this approach can be successfully used for determination of Cd(II) in water samples.     

Electrochemical investigation and determination of ceftazidime in pharmaceutical dosage forms and human urine

A voltammetric study of the oxidation of Ceftazidime (CEFT) has been carried out at the glassy carbon electrode by cyclic, differential pulse (DPV) and square wave (SWV) voltammetry. The oxidation of CEFT was irreversible and exhibited diffusion controlled process depending on pH. The oxidation mechanism was proposed and discussed. According to the linear relationship between the peak current and concentration, DPV and SWV voltammetric methods for CEFT assay in pharmaceutical dosage forms and human urine were developed. For analytical purposes, a well resolved diffusion controlled voltammetric peak was obtained in 0.1 M H₂SO₄ at 1.00 and 1.02 V for differential pulse and square wave voltammetric techniques, respectively. The linear response was obtained within the range of 4 × 10^?6?8 × 10^?5 M with a detection limit of 6 × 10^?7 M for differential pulse and 4 × 10^?6–2 × 10^?4 M with a detection limit of 1 × 10^?6 M for square wave voltammetric technique. The determination of CEFT in 0.1 M H₂SO₄ was possible over the 2 × 10^?6–1 × 10^?4 M range in urine sample for both techniques. The standard addition method was used for the recovery studies.     

Ultrasound-assisted ozone bleaching of cotton

In this study, the effects of ultrasound on ozone treatment processes for bleaching cotton fabrics were investigated and compared with the conventional hydrogen peroxide bleaching process (60 °C over 90 min). Two ultrasonic + ozone treatments of cotton fabric samples were carried out: (1) ozone in an ultrasonic homogenizer (UH) and (2) ozone in an ultrasonic bath. Ozone dosages, temperature and time variations were determined with both ozone-ultrasonic bleaching processes. Whiteness, yellowness, weight, tensile strength properties, FTIR (ATR) spectra and visual appearance, via scanning electron microscopy of treated cotton fabrics as well as chemical oxygen demand (COD) of bleaching effluents, were investigated. It was concluded that the ozone + UH process, conducted for 30 min at 30 °C, produced closely equivalent values of cotton fabric whiteness and yellowness to the classic peroxide bleaching process, with slightly less weight loss, dramatically less COD in the process effluent (29 mg/l for ozone-UH vs. 4,316 mg/l for classical peroxide treatment), and without causing any adverse and/or detrimental effects on loss of fabric strength or elongation of the cotton fabrics. The ozone-UH process also leads to time and energy savings with much less environmental impact. Consequently, the combination of ozonation plus UH carried out at 30 °C over 30 min can be used successfully for cotton bleaching instead of the classic hydrogen peroxide bleaching process.     

Sensitive Nucleic Acid Detection at NH2‐MWCNTs Modified Glassy Carbon Electrode and its Application for Monitoring of Gemcitabine‐DNA Interaction

An electrochemical dsDNA nanobiosensor was fabricated using amino‐functionalized multi walled carbon nanotubes modified glassy carbon electrode (NH₂fMWCNTs/GCE) for the sensitive detection of DNA bases and electrochemical monitoring of drug‐DNA interaction. The influence of functional groups on MWCNT was studied by MWCNT functionalized with NH₂ (NH₂fMWCNTs) and COOH (COOHfMWCNT) groups based on the signal of DNA bases. The modified electrodes were characterized by scanning electron microscopy. One layer of calf thymus double stranded deoxyribonucleic acid (ct‐dsDNA) was immobilized onto the NH₂fMWCNTs/GCE (dsDNA/NH₂fMWCNTs/GCE). The dsDNA/NH₂fMWCNTs/GCE were used to investigate the interaction between the dsDNA and the anticancer drug gemcitabine by differential pulse voltammetry in acetate buffer of pH 4.70. For the confirmation of interaction, the lowering in intensity of the current signals of guanine and adenine was considered as an indicator. Electrochemical impedance spectroscopy studies were performed for the comparison of the modified surfaces. In order to define and visualize the interaction mechanism between gemcitabine and dsDNA/NH₂fMWCNTs/GCE at the molecular level, in silico methods including docking and molecular dynamics simulations were employed.     

Synthesis,optical, and structural properties of bisphenol-bridged aromatic cyclic phosphazenes

Phenoxy- and naphthoxy-substituted bisphenol-bridged cyclic phosphazenes were synthesized in 2 steps and their thermal, photophysical, and electrochemical properties were investigated. The structures of the cyclic phosphazene compounds were determined by ESI-MS mass spectrometry and ¹ H, ¹³ C, and ³¹ P NMR spectroscopies. The photophysical studies of phenoxy- and naphthoxy-substituted bridged cyclophosphazenes were investigated by means of absorption and fluorescence spectroscopies in different solvents. Thermal and electrochemical properties of the target compounds were also studied. Furthermore, the excimer emissions through intramolecular interactions in solution and in solid state were investigated by fluorescence spectroscopy and the theoretical calculations were performed in detail using DFT.     

Experimental investigation of the effects of length to diameter ratio and nozzle number on the performance of counter flow Ranque–Hilsch vortex tubes

In this experimental study, performance of counter flow type Ranque-Hilsch vortex tubes (RHVT), with a length to diameter ratio of 10, 15 and 18, were investigated with 2, 4, 6 nozzles. The measure of performance was chosen as the difference between the temperatures of hot output stream and cold output stream. The performances of RHVTs were experimentally tested by making use of velocity and temperature measurements of the input and output streams. It was determined that the difference between the temperatures of these streams, changed between 9 and 56 K. When all the results were assessed, it was concluded that the best performance was obtained when the ratio of vortex tube’s length to the diameter was 15 and the nozzle number was at least four, and the inlet pressure was as high as possible. Desired performance could be obtained by controlling the rate of the hot output stream.     

Synthesis and investigation of antibacterial activities and carbonic anhydrase and acetyl cholinesterase inhibition profiles of novel 4,5-dihydropyrazol and pyrazolyl-thiazole derivatives containing methanoisoindol-1,3-dion unit

Novel 4,5-dihydropyrazole derivatives (3a–i), 3-(4-((3aR,4S,7R,7aS)-1,3-dioxo-3a,4,7,7a-tetrahydro-1H-4,7-methanoisoindol-2(3H)-yl)phenyl)-5-phenyl-4,5-dihydro-1H-pyrazole-1-carbothio amide, were obtained by the addition of thiosemicarbazide (2) to the chalcones (1a–i). The addition–cyclization of 2,4′-dibromoacetophenone (4) to pyrazole derivatives (3a–i) gave the new pyrazolyl-thiazole derivatives (5a–i), (3aR,4S,7R,7aS)-2-(4-(1-(4-(4-bromophenyl)thiazol-2-yl)-5-phenyl-4,5-dihydro-1H-pyrazol-3-yl)phenyl)-3a,4,7,7a-tetrahydro-1H-4,7-methanoisoindole-1,3(2H)-dione. Antibacterial and acetylcholinesterase (AChE) enzyme and human carbonic anhydrase (hCA) I, and II isoform inhibitory activities of the compounds 3a–i and 5a–i were investigated. Some of the compounds showed promising antibacterial activity. In addition, the hCA II and I were effectively inhibited by the lately synthesized derivatives, with K_i values in the range of 18.90?±?2.37 ?58.25?±?13.62?nM for hCA II and 5.72?±?0.98 ?37.67?±?5.54?nM for hCA I. Also, the K_i parameters of these compounds for AChE were obtained in the range of 25.47?±?11.11???255.74?±?82.20?nM. Also, acetazolamide, clinical molecule, was used as a CA standard inhibitor that showed K_i value of 70.55?±?12.30?nM against hCA II, and 67.17?±?9.1?nM against hCA I, and tacrine inhibited AChE showed K_i value of 263.67?±?91.95.     

Efficient one-pot three-component method for the synthesis of highly fluorescent coumarin-containing 3,5-disubstituted-2,6-dicyanoaniline derivatives under microwave irradiation

A simple and concise approach to the synthesis of coumarin-containing highly fluorescent asymmetric/symmetric 3,5-diaryl/heteroaryl-2,6-dicyanoaniline derivatives are reported. The compounds were synthesized through base catalyzed three-component one-pot synthesis reaction of 2-(1-(7-(diethylamino)-2-oxo-2H-chromen-3-yl)ethylidene)malononitrile, aliphatic, aromatic/heteroaromatic aldehydes, and malononitrile in solvent-free reaction medium, catalyzed by piperidine under microwave irradiation method. The reaction gave the novel, highly fluorescent coumarin-containing 3,5-disubstituted-2,6-dicyanoaniline derivatives in good yields at 300?W, 80?°C in 2?min. This method provides several advantages; such as shorter reaction time, environmental friendliness, simple workup procedure, lower energy consumption and, generally, good yields with high purity. In addition, the synthesized compounds are fluorescently active dyes even in day light, except for compounds including nitro substituent, and show maximum absorption wavelengths (λ_abs.max) in the visible region in DMSO at room temperature. Thermal properties of all the synthesized compounds were also evaluated with thermal gravimetric analysis for usability as optic dye. Optical and thermal screening studies of the compounds showed that the dyes have excellent photophysical and thermal stability properties.