In this study, the preparation of novel 7-hydroxy-3-(2-chloro-4-fluorophenyl)coumarin (1), the ligand, 7-(3,4-dicyanophenoxy)-3-(2-chloro-4-fluorophenyl)coumarin (2), metal-free phthalocyanine 3 and metallophthalocyanine complexes 4 and 5 (MPcs, M = Co, Zn), β-substituted with 7-oxo-3-(2-chloro-4-fluorophenyl)coumarin functional group was achieved. By the reaction of 7-hydroxy-3-(2-chloro-4-fluorophenyl)coumarin (1) with 1,2-dicyano-4-nitrobenzen in dry DMF as the solvent in the presence of K2CO3 as the base, the 7-(3,4-dicyanophenoxy)-3-(2-chloro-4-fluorophenyl)coumarin (2) was synthesized. Compound 2 reacted with Co(CH3COO)2·4H2O in 2-N,N-dimethylaminoethanol to furnish a novel coumarin containing cobalt(II) phthalocyanine 4. The cyclotetramerization of 2 with Zn(CH3COO)2·2H2O in 2-N,N-dimethylaminoethanol gave the novel coumarin containing Zn(II)phthalocyanine 5; while tetramerization without any metal salts in 2-N,N-dimethylaminoethanol gave the metal-free phthalocyanine 3. The structures of obtained compounds were confirmed by elemental analysis, UV–Vis, IR, MALDI-TOF mass and 1H NMR spectra. The cyclic and differential pulse voltammetry, and in situ spectroelectrochemistry of 7-oxo-3-(2-chloro-4-fuorophenyl)coumarin substituted phthalocyanines 3, 4 and 5 allowed us to identify metal- and phthalocyanine ring-based redox processes of the complexes. 相似文献
Calixarenes, which have a great place in supramolecular chemistry, have become the most prominent macrocyclic compounds in synthetic organic chemistry due to their easy synthesis and functionalization. In this study, p-tert-butyl calix[4]arene dihydrazide derivative was synthesized and then reacted with 3-oxo-3,4-dihydro-2 H-benzo[b][1,4] thiazin-2-ylideneacetyl chloride to prepare new calixarene based chromophore compound 4. The structure of the synthesized compound was elucidated by spectroscopic methods such as 1H NMR 13C NMR and FT-IR spectroscopy. Chromogenic and fluorescence properties of compound 4 were evaluated. It was observed from both studies that compound 4 was Co2+ selective and shows fluorescence Switched-off behavior. Stoichiometry, binding constant and the detection limit were calculated. The stoichiometry between compound 4 and Co2+ was found to be 1:1. The binding constant value (K) was calculated as 666.67 M??1 using Benesi–Hildebrand equation, while the detection limit for Co2+ ion was calculated as 0.0465 µM.
This study is interested in the effect of lithium carbonate on the formation of hexagonal boron nitride (hBN) by means of the available experimental methods including TGA, XRD, FTIR, SEM and HR‐TEM. hBN samples were synthesized at the 1450 °C with different molar ratios of lithium carbonate by modified O'Connor routine. The crystalline hBN formation tended to improve with the increment of the Li2CO3 concentration level (especially after more 20 %). The dopant quantity decreased the residual stresses due to the presence of possible relaxation mechanisms along with the nanocrystal structure, even favored by XRD experimental findings regarding the enhancement of crystal plane alignments, crystallite sizes and lattice parameters. As for the FTIR surveys, the Li2CO3 foreign impurities strengthened more and more the covalent bonds between boron and nitrogen atoms. At the same time, the samples with 40 % lithium carbonate were annealed at the varied temperatures of 1000, 1150, 1300 and 1450 °C to determine the optimum annealing temperature. The XRD+FTIR investigations indicated that the degree of hexagonality improved with the increased annealing temperature. Similarly, the surface morphology confirmed not only the formation of regularity and flaky hexagonal BN structures, but also the strengthening of covalent bonds between the atoms. 相似文献
Tannic acid (TA) complexes with various metal ions are prepared in buffer solutions by readily adjusting the pH, but there is no normalizing method to produce ferric tannate complexes. In this study, TA-Fe(III) complex was prepared in reverse microemulsion medium by reaction of TA as ligand with Fe(III) in 1:3 ligand:metal ion molar ratio. The complex was characterized by SEM, AFM, FT-IR, elemental analysis, AAS measurement, and Brunauer-Emmett-Teller (BET) method. Furthermore, magnetic susceptibility was tested with the Gouy method, and electronic spectral studies of TA-Fe(III) complex were completed with solid UV–vis measurements. The thermal stability was also studied by TGA analysis. These studies show that the ligand molecules have octahedral arrangement around Fe(III) and the complex is paramagnetic. The bandgap energy of the complex was calculated as 3.42 eV with solid UV–vis analysis. To determine antioxidant activity of the complex, Total Phenol Content (TPC) and Trolox Equivalent Antioxidant Concentration (TEAC) methods were used. The complex has great antioxidant properties with TPC = 45 ± 1 mg L?1 GAE and TEAC = 296 ± 2 mM trolox g?1 for dry sample. 相似文献
The current study focuses on the synthesis and sorption properties of two mixed oxides of iron and silicon prepared by physical mixing (M1) and sequential precipitation methods (M2). Both the mixed oxides were synthesized from equimolar ratios of Fe(OH)3 and SiO2 and characterized for surface area, EDX, XRD and PZC. The surface area, micropore volume and average pore width of the oxide M1 were higher as compared to the oxide M2. However, potentiometric titrations revealed that mixed oxide synthesized by this method had a very high capacity towards Cd2+ ions as compared to the mixed oxide M1. Sorption of Cd2+ ions at pH 5 on mixed oxide, M2 was found to increase with temperature in the range 288 to 318 K. Langmuir equation was found applicable to the sorption data with R2>0.99. Entropy (ΔS?), enthalpy (ΔH?) and free energy changes (ΔG?) were calculated which revealed the process to be endothermic and spontaneous in nature. 相似文献
Chromium(III) sorption on macroporous strong cation exchanger Amberlyst‐15 (H+) was studied as a function of time and temperature. The rate constant values for chromium(III) sorption were calculated both for film and particle diffusion processes. The temperature was found to have a positive effect on both the diffusional processes. From the rate constant values, the energy of activation was calculated using the well‐known Arrhenius equation. The high values of energy of activation confirmed the film diffusional nature of the process. Equilibrium data were explained with the help of Langmuir equation. Various thermodynamic parameters (ΔH?, ΔS? and ΔG?) from chromium(III) exchange on the resin were calculated. The ΔG? values were found to be negative while both the ΔH? and ΔS? were positive. 相似文献
Possible stable conformers of the 1-(4-pyridyl)piperazine (1-4pypp) molecule were experimentally and theoretically studied
by FT-IR and Raman spectroscopy. FT-IR and Raman spectra were recorded in the region of 4000–200 cm−1. Optimized geometric structures related to the minimum on the potential energy surface were investigated by the B3LYP hybrid
density functional theory method using the 6-31G(d) basis set. Comparison of the experimental and theoretical results indicates that the density functional B3LYP method provides
satisfactory results for the prediction of vibrational wavenumbers and structural parameters and equatorial-equatorial (e-e) isomer is supposed to be the most stable form of the 1–4pypp molecule. 相似文献