In this study, for the first time Brij 58 was used for the spectrophotometric determination of sunset yellow (SY) (E-110) in pharmaceutical preparations and powdered beverages after cloud point extraction (CPE). Certain parameters such as pH, surfactant concentration, extraction time and temperature, centrifuge speed and salt concentration were optimized. Linear range in the optimum conditions was 0.01 – 4.00 mg mL-1 and the correlation coefficient was 0.9995. The limit of detection (LOD) and the limit of quantification (LOQ) of this method were 0.0078 mg mL-1 and 0.0261 mg mL-1, respectively.

Two samples of Tanacetum praeteritum (Horwood) Heywood subsp. praeteritum (Horwood) were collected in flowering period and subjected separately to hydrodistillation to yield the essential oils (A and B). The oils were investigated for chemical composition with GC-FID and GC/MS techniques and evaluated against acetylcholinesterase and a-amylase enzymes and free radicals (DPPH• and ABTS•+) using microtiter plate assays. Both of the oils were characterized with high abundance of oxygenated monoterpenes. The oils were distinguished by the main constituents, namely, camphor (37.6 %), 1,8-cineole (19.5 %) and terpinen-4-ol (9.3 %) were found as the major constituents in the oil A, while a-thujone (79.4 %) and b-thujone (8.5 %) were detected in the oil B. The oils demonstrated significant inhibitory (80 % and 60.0 %) potentials on acetylcholinesterase (an IC50 of 0.74 mg/mL and an IC50 of 1.78 mg/mL, respectively) which involved into Alzheimer’s disease. With respect to antidiabetic activity, the oils demonstrated significant inhibiting potential on porcine pancreatic a-amylase (an IC50 of 1.02 mg/mL and an IC50 of 0.89 mg/mL) in I2/KI assay. The oils demonstrated weak free radical scavenging activity against DPPH radicals and moderate activity (0.23 mM and 0.15 mM) against ABTS+• in TEAC assay.

Novel precursors were developed for deposition of Cu and Pd nanoparticles on multiwalled carbon nanotubes for supercritical carbon dioxide deposition technique. 3-(heptadecafluorooctyl)aniline-vic-dioxime and phenanthrenequinonedioxime were used as ligands in synthesis of the palladium and copper precursors. All synthesized ligands and complexes were characterized with elemental analysis, 1H and 19F NMR, FT-IR and magnetic susceptibility technique. Deposition of these precursors in supercritical carbon dioxide was performed at 363ºK in the pressure 0.69 MPa H2 and 27.6 MPa CO2. Surface morphology of metal deposited multiwalled carbon nanotubes has been investigated with X-ray diffraction, high-resolution transmission electron microscopy and scanning electron microscopy with EDX. TEM micrographs showed homogenous distributions of Cu and Pd nanoparticles on the multiwalled carbon nanotubes. The nature and crystallinity of the nanoparticles were confirmed using XRD. This study showed that these novel vic-dioxime complexes are suitable precursors for the preparation of supported metal nanoparticles in supercritical carbon dioxide.

Metallic corrosion is one of the most important problem in various industrial fields. One of the most effective methods to deal with metallic corrosion is to design and use appropriate organic corrosion inhibitors. In the present study, various amide-based, sulfur-containing nonionic surfactants were synthesized and characterized by spectroscopic methods. The corrosion inhibition properties of these synthesized compounds were investigated. For this purpose, mild steel coupons were immersed for 24 hours at room temperature in 1 M HCl containing different concentrations of inhibitor according to the ASTM NACE / ASTMG31-12a standart method. As a result of these corrosion tests, the synthesized compounds exhibited very good inhibitory properties (76.58-93.74 IE%). Surface characterization studies were also performed for the metal coupons to support the obtained corrosion inhibition efficiency results.

The increase in multidrug resistance malaria cases necessitates the need to search for new cost effective drugs. QSAR and molecular docking studies were performed on a data set of forty nine Pyrrolones antimalarial agents against Plasmodium falciparum. Forty two molecules were used as training set and seven as test set. The molecular descriptors were obtained by Density Functional Theory (DFT) (B3LYP/6-31G**) level of calculation. The QSAR model was built using Genetic Function Algorithm (GFA) method. The model with the best statistical significance (N = 42, R2ext = 0.700, R2 = 0.933, R2a = 0.916, Q2cv = 0.894, LOF = 0.417, Min expt. error for non-significant LOF (95%) = 0.250 was selected. The docking experiment was carried out using AutoDock Vina of PyRx and Discovery Studio Visualizer. Docking analysis revealed that three of the studied compounds with binding affinity values of -10.7 kcal/mol, -10.9 kcal/mol and -11.1 kcal/mol possess higher potency than standard antimalarial drugs with binding affinity of values of -8.8 kcal/mol, -9.5 kcal/mol and -9.0 kcal/mol. It is envisioned that the wealth of information provided by the QSAR and molecular docking results in this study will offer important structural insights for further laboratory experiments in the future design of novel and highly potent antimalarial from Pyrrolones.

Thymelaea microphylla Coss. et Dur is an endemic desert species from Algeria belongs to Thymelaeaceae family. The dichloromethane-methanolic extract from aerial parts of T. microphylla was subjected to silica gel column. Three flavonoids were isolated from the extract; isochamaejasmin (1), cis-tiliroside (2) and trans-tiliroside (3). The structures of the compounds were determined on the basis of the HPLC-TOF/MS, 1D and 2D NMR spectroscopic analysis. To the best of our knowledge, compound (1) was isolated from T. microphylla for the first time and there is no report in the literature. Moreover, in this study, antioxidant activity of the compound (3) was also evaluated.

This article presents a simple and practical method for the synthesis of 3,4-dihydropyrano[c]chromene, which are heterocyclic compounds possessing a wide range of biological properties. They have been obtained by the condensation of an aromatic aldehyde, malononitrile and 4-hydroxycoumarin in presence of phosphate fertilizers (MAP, DAP and TSP) as heterogeneous catalyst and ethanol as an ecological solvent that makes this procedure environmentally friendly. The aim of this study is the investigation of their catalytic activities through the determination of the optimum conditions, which are the reaction time, the mass of the catalyst used, the nature of the solvent and its appropriate volume. These optimum conditions are the mean ones in the catalytic efficiency and they permit to obtain better yields with shorter reaction times. The developed method herein presents a green strategy which is characterized by mild reaction conditions, high to excellent yields, short reaction times and easy catalyst recovery. In addition, the experiment shows that these catalysts can be reused successfully several times without significant loss of their catalytic activity.

The aim of this research is to synthesize and characterize of new cyclic members of cyclic aminobenzoquinones. Mono amino substituted products; 2-chloro-5,6-dimethyl-3-(pyrrolidin-1-yl)-1,4-benzoquinone (2), 2-chloro-5,6-dimethyl-3-(piperidin-1-yl)-1,4-benzoquinone (3), 2-chloro-5,6-dimethyl-3-morpholino-1,4-benzoquinone (4), and 2-chloro-5,6-dimethyl-3-thiomorpholino-1,4-benzoquinone (5) have been synthesized by a green methodology using water as solvent by means of nucleophilic substitution reactions between 2,3-dichloro-5,6-dimethyl-1,4-benzoquinone (1) and cyclic secondary amines. Structure determination of the new products (2-5) was established on the basis of IR, 1H NMR, 13C NMR, and mass spectrometry.

The present study describes the use of pencil graphite electrode (PGE) for the investigation of electro-oxidation mechanism and voltammetric stripping determination of dasatinib (DST) in Britton-Robinson buffer solution (BR). Relating to cyclic voltammetric studies, an irreversible oxidation signal was obtained at about 1.0 V. The oxidation electrode process is adsorption-controlled and pH-dependent. For quantitative determination of DST, square wave adsorptive stripping voltammetry (AdsSWV) was employed in BR of pH 3.0. The oxidation peak current varies linearly with the DST concentration in the range of 0.0092 – 1.0 µM. Dedection (LOD) and quantification (LOQ) values are founded as 0.0028 µM and 0.0092 µM, respectively. The developed AdsSWV method based on disposible and cheap PGE was applied successfuly to the real urine samples and the recovery results are given in the range of 97.94% to 100.82%.

Two new coordination polymers, namely [Mn(µ3-5-nip)(1-meim)2(H2O)]n (1) and {[Co(µ-5-nip)(1-meim)3]·H2O}n (2) (5-nip: 5-nitroisophthalate, 1-meim: 1-methylimidazole), were hydrothermally synthesized and characterized by IR spectroscopy, elemental analysis, single crystal diffraction and simultaneous thermal analysis techniques. The 5-nip ligand exhibited two different coordination modes in its structures. In 1 and 2, 1D chains were generated by 5-nip ligands and metal (II) ions. In 1 and 2, 5-nip ligand coordinated to three Mn(II) and two Co(II) ions as bis(monodentate) bridging mode and a monodentate and bidentate chelating modes, respectively. For 1 and 2, 2D supramolecular layers were formed by hydrogen bonds which were extend into 3D supramolecular structures via p···p interactions between two symmetry–related imidazole rings of neighboring molecules. Furthermore, optical and thermal properties of the complexes were also studied.

Amine (2) and (26) was obtained from the condensation of the corresponding amines with 3,4-difluoronitrobenzene. The reduction of nitro group produced the corresponding amines (3 and 27). The synthesis of esters (7, 12, 19, 28) was carried out from the treatment of the amines, 1, 3, 18, 27 with ethylbromoacetate, then these compounds were converted to the corresponding hydrazides (8, 13, 29) by the treatment with hydrazine hydrate. Triazole was obtained from the intramolecular cyclisation of the corresponding carbothioamide in basic media and this compound wad then converted to the morpholine-triazole-penicillin hybrid by a mannich reaction. The cyclocondensation of hydrazine carbothioamides (9b, 14, 21) or urea (4) with 2-bromo-1-(4-chlorophenyl) ethenone generated thiazole derivatives. On the other hand, the treatment of 4, 9b and 14 with ethyl bromoacetate yielded 4-oxo-1,3-thiazolidines (6, 11, 16). Three methods containing conventional, microwave and ultrasound mediated techniques were applied. Best results were assessed using microwave and ultrasounds promoted procedures. All the newly synthesized compounds were characterized on the basis of spectroscopic techniques, and they were screened for their antimicrobial activity. Some of them exhibited good-moderate activity on the test bacteria.

This study is about preparation of two different organoclays with cationic surfactants and their poly(vinyl alcohol) nanocomposites with increased thermal and mechanical behavior. Organoclays were prepared modifying clay mineral with solution intercalation method using aqueous solutions of cationic surfactants dodecyltrimethylammonium bromide (DTABr) and cetylpyridinium bromide (CPBr). Obtained organoclays (D-MMT and C-MMT for DTABr/MMT and CPBr/MMT, respectively) were characterized using different methods including zeta potential and XRD. Results indicated an absolute decrease in zeta potential about 20 mV for C-MMT, and 14 mV for D-MMT indicating flocculation and coating of the surface. Moreover measurements indicated that interlayer distance increased based on basal spacing peak shift whose value was 1.27 nm for NaMMT, whereas 1.40 nm for D-MMT, and 1.75 nm for C-MMT. The organoclays were used in preparation of PVA/clay nanocomposites; thermal stability of the nanocomposites were determined using TGA, while mechanical strength measurements were done using DMA. Maximum thermal decomposition temperature of the pristine PVA and nanocomposites were compared and an average increase of 4°C were observed. Also activation energy of the decomposition was observed ca. 40 kj mol-1 higher than pristine PVA.

In this work, a convenient protocol enabled the synthesis of novel Arylated Borondipyrromethene (BODIPY) compounds was applied that synthesis yields found to be higher than classical alkyl substituted analogue. Arylated chromophores exhibited the broader red-shifted absorption and fluorescence bands with higher stokes shifts with regard to reference Borondipyrromethene compound (4,4’-difluoro-8-phenyl-1,3,5,7-tetramethyl-4-bora-3a,4a-diaza-s-indacene,). We interested in the electron transfer mechanism of compound BDPNH2 which have amine subunit to alkyl substituted reference. The fluorescence enhancement of this compound in acidic media was associated with the inactivation of the acceptor type photoinduced electron transfer mechanism by fluorimetric measurements. Our results are helpful for designing new photosensitizers and for applications in the study of the molecular photochemistry.

In this study, we prepared nine Schiff bases by condensation of amino acid methyl esters (isoleucine, phenylalanine and methionine) with salicylaldehyde derivatives (2,4-dihydroxybenzaldehyde, 2-hydroxy-3-methoxybenzaldehyde and 5-bromo-2-hydroxybenzaldehyde) and characterized by various spectroscopic methods (FT-IR, UV-Vis and NMR techniques). FT-IR and UV-Vis spectra exhibited characteristic peaks for all imine compounds. NMR spectra pointed out the imine bond which is the indicator of the formation of Schiff bases. Besides, antiproliferative and cytotoxic features of the Schiff bases were examined by using MTT cell proliferation and LDH cytotoxicity assays, respectively. Amongst the synthesized Schiff bases, compound 3d exhibited a very strong antiproliferative effect against all cells except A549. The experimental studies revealed that the Schiff bases synthesized in this study, especially 3d, have an important potential to enter drug development studies.

In present study, we report phenolic compounds and antioxidant activity of decoction and infusion of Mentha spicata L. subsp. spicata and M. longifolia (L.) L. subsp. typhoides (Briq.) Harley. The quantitative amounts of the phenolic contents were determined by LC-MS/MS. The main compounds and amounts of M. spicata were determined as follow for decoction; caffeic acid, quercetagetin-3,6-dimethylether and penduletin (4126.6; 2141.5; 1472.7 mg/kg dried herba, respectively), for infusion; fumaric acid, t-ferulic acid and caffeic acid (4220.1; 1148.7; 1064.1 mg/kg dried herba, respectively). While phenolic compounds in M. longifolia decoction were presented as follow; rosmarinic acid, luteolin and quercetagetin-3,6-dimethylether (1570.7; 460.9; 420.2 mg/kg dried herba, respectively), for infusion; rosmarinic acid, luteolin and fumaric acid (620.9; 518.2; 489.8 mg/kg dried herba, respectively). Also the antioxidant activities were determined based on three methods: 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging, ß-carotene linoleic acid assays and cupric (Cu2+) ion reducing power assay (CUPRAC). For all the activity assays, infusion and decoction of the samples showed good activity.

Peptide nucleic acids are synthetic molecules crafted to mimic natural nucleic acids, and thus, they are widely utilized in many chemical, and, biomedical applications. Although there exist many approaches to synthesize monomers to date, there is still room to improve these methodologies. With this motivation, we compared some widely utilized synthetic routes to obtain N-Boc-PNA-T-OH, and N-Fmoc-PNA-T-OH. Our results indicate that N-Boc-ethylenediamine is the most pivotal intermediate in the chemistry of PNA, and synthetic route commencing with this material affords these two PNA monomers in relatively high yield, and purity, while being very reproducible.

A new polymerization mechanistic transformation strategy, combining two different controlled polymerization techniques of different modes, atom transfer radical polymerization (ATRP) and photoinduced radical oxidation/addition/deactivation (PROAD), is successfully applied for the synthesis of block copolymers. Thus, mono- or bi- bromide functional polystyrenes (PS-Br or Br-PS-Br) synthesized by light induced ATRP were used as macroinitiator for the living cationic polymerization of isobutyl vinyl ether via PROAD process to give the corresponding block copolymers. In this way, depending on the structure of the macroinitiator, AB or ABA type block copolymers (PS-b-PIBVE or PIBVE-b-PS-b-PIBVE) were formed. The final polymers and precursor polymers were characterized by spectral and chromatographic analyses.

Amidoxime modified ethyl cellulose (EC-g-AO) was used for the recovery of uranyl ions from aqueous solutions by a complexation process. Adsorption trials were carried out in different concentrations of UO22+ solutions (100 – 1000 mg/L) and at temperatures ranging from 25 to 50°C. The kinetics and the thermodynamics of the adsorption of uranyl ions (UO22+) by EC-g-AO were investigated. The adsorption capacity was found as 240 mg UO22+/g dry copolymer. The thermodynamic parameters for the interaction of UO22+ with EC-g-AO were calculated from thermodynamic relations. Calculations showed that adsorption occurred through strong electrostatic interactions with an enthalpy of -23.6 kJ/mol. The desorption of UO22+ was investigated by desorption agents like EDTA, HCl, NaHCO3, and NaOH. 52 % of desorption yield was found for NaHCO3.

Successive reaction of long chain w-1, w-2, w-4 and w-5 hydroxycarboxylic acids 1a-1e with a cyanuric chloride (CC) and triethylamine afforded the corresponding racemic lactones 2a-2e in high yields. Optically pure R lactones 4a-4e were synthesized stereoselectively by porcine pancreas lipase-catalysed resolution of racemic 2a-2e. The resolution conditions were investigated, determined and optical rotations were measured. The mentioned chiral lactones were synthesized by this method for the first time. The obtained racemic and chiral lactones were analysed by NMR, IR, Mass, optical rotation and C,H analysis.

In this work, 15 different coumarin hydrazides were successfully synthesized and screened for their antioxidant and antilipase activities. To do this, firstly, salicylaldehyde derivatives and 2,2-dimethyl-1,3-dioxane-4,6-dione (Meldrums Acid) were reacted in ethanol in the presence of catalytic amount of pyridine to obtain coumarin-3-carboxylic acid derivatives (1a-e). Then, these compounds were treated; with benzotriazole in dichloromethane by using thionyl chloride to synthesized benzotriazole derivatives (2a-e). Then, compounds 2a-e were reacted; with three commercial hydrazides (nicotinic hydrazide, benzhydrazide and phenylacetichydrazide) in ethanol by using microwave irradiation and conventional heating procedures to obtain final products (3-5a-e). Finally, these compounds were tested for their anti-oxidant and anti-pancreatic lipase activities. The structure of newly synthesized compounds was identified by 1H NMR, 13C NMR and elemental analysis data.

In this study, amine-mediated silica aerogels dried under the ambient conditions in monolithic form were prepared by following sol-gel method. 3-aminopropyltriethoxysilane (APTES) was involved to the synthesis as a silica co-precursor. Imidazolium based short-chain ionic liquids (ILs) were incorporated into the silica gel structure to control the gel shrinkage within the pores, as well as to eliminate the capillary effect during the solvent evaporation. A production procedure was developed to explore the synergistic effect of ionic liquids and amine functionalized silica precursor on the textural and chemical properties of the final silica gels. Surface modifications of the samples were performed by using 3-Methacryloxypropyltrimethoxysilane (MEMO) to ensure hydrophobic characteristics. To reveal the chemical and morphological characteristics of the resultant material, various analyses were conducted. SEM and FTIR analyses were performed to investigate the morphological and chemical structure, whereas TGA analysis was carried out to determine the thermal stability of the silica gels. As a result, ionic liquid embedded sample was obtained in a monolithic structure with a low density (0.45 g/cm3) and had a good thermal stability (up to 381 °C). Contact angle measurement also demonstrated that the desired monolithic sample has hydrophobic characteristic with a water contact angle value of 113°.

The economic synthesis of quinaldinium chlorochromate(VI), C10H9NH[CrO3Cl], (QnCC) was performed by using a 1:1:1 stoichiometric amounts of CrO3, HCl (aq) and quinaldine. QnCC was isolated in 99% yield as an orange crystalline solid and characterized with FT-IR, 1H-NMR, and 13C-NMR. An efficient, selective, and environmentally friendly oxidation of alcohols with 1.1 equiv. periodic acid (H5IO6) catalyzed by QnCC (2 mol%) is described. The primary and secondary alcohols were oxidized to their corresponding aldehydes and ketones under solvent-free conditions at room temperature and MW irradiation in high to excellent yields.

In the present study, the optimum conditions have been investigated for the separation of Zn2+ ions from aqueous media by micellar enhanced ultrafiltration (MEUF). For this purpose, optimum conditions for the concentration of surface active agent in the feed solution (sodium dodecyl sulfate, SDS), cetyltrimethyl ammonium bromide (CTAB), triton-X-100 (TX100)), filtering pressure, stirring rate and for the membrane porosity have been determined. It is shown that the filtering pressure has a significant effect on the permeate flux but a relatively insignificant impact on rejection of Zn2+. Permeate flux increased linearly with increasing pressure, ranging from 0.32 mLmin-1m-2 at 3 bar to 0.72 mLmin-1m-2 at 4 bar. The results showed that by adding SDS anionic surfactant, the permeate flux and the removal efficiency of zinc increased. Best results in terms of zinc rejection coefficient is 97.5 % at 5.0 x 10-4 M zinc concentration, 1.0 x 10-2 M SDS concentration (~x 8 cmc), stirring rate 500 rpm and transmembrane pressure 4 bar.

Chlorotoxin (CLTX) is a neurotoxin found in the venom of the Israeli scorpion, Leirius quinquestriatus. It contains 36-amino acids with four disulfide bonds and inhibits low-conductance chloride channels. CLTX also binds to matrix metalloproteinase-2 (MMP-2) selectively. The synthesis of chlorotoxin using solid phase peptide synthesis (SPPS) is very difficult and has a very low yield (<1%) due to high number of amino acid sequence. In this work, to improve the efficiency of the synthesis, native chemical ligation was applied. In this strategy, chlorotoxin sequence was split into two parts having 15 and 21 amino acids. 21-mer peptide was synthesized in its native form based on 9-fluorenylmethyloxycarbonyl (Fmoc) chemistry. 15-mer peptide was synthesized having o-aminoanilide linker on C-terminal. These parts were coupled by native chemical ligation to produce chlorotoxin.

In this paper, terpenic metabolites of Tanacetum abratonifolium are reported. Eight known sesquiterpene lactones: tanachin (1), tavulin (2), tamirin (3), spiciformin (4), isospiciformin (5), 1ß-hydroxy-6a-angeloxy-oxygermacra-4(5),10(14),11(13)-trien-8,12-olide (6), dentatin A (7), 1-ß-hydroxy-6a-angeloyloxyeudesm-4(15), 11(13)-dien-8,12-olide (8) as well as a-amyrin (9) and ß-sitosterol (10) were isolated from the aerial parts of Tanacetum abratonifolium, collected in East Turkey.