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1.
A new (E,E)-dioxime, (6Z,7Z)-15,16-dihydro-14H-dibenzo[b,h][1,10,4, 7]dithiadiazacyclotride-cine-6,7(5H,8H)-dionedioxime (H
2
L) has been synthesized by reacting cyanogen-di-N-oxide (2) with 2,2′-[propane-1,3-diylbis(thio)]dianiline (1). Mononuclear complexes (4) and (5) of this ligand have been synthesized by reacting the vic-dioxime (H2L) with NiCl2 · 6H2O and CoCl2 · 6H2O, respectively. The BF
2
+
capped Ni(II) and Co(III) complexes (6) and (7) of the dioxime have been synthesized from (4) and (5). The new compounds were characterized by a combination of elemental analysis, 1H- and 13C-n.m.r, i.r. and m.s. spectral data. 相似文献
2.
New 3,3‐diphenylpropoxyphthalonitrile (5) was obtained from 3,3‐diphenylpropanol (3) and 4‐nitrophthalonitrile (4) with K2CO3 in DMF at 50 °C. The novel cobalt(II) phthalocyanine complexes, tetrakis‐[2‐(1,4‐dioxa‐8‐azaspiro[4.5]dec‐8‐yl)ethoxy] phthalocyaninato cobalt(II) (2) and tetrakis‐(3,3‐diphenylpropoxy)phthalocyaninato cobalt(II) (6) were prepared by the reaction of the phthalonitrile derivatives 1 and 5 with CoCl2 by microwave irradiation in 2‐(dimethylamino)ethanol for at 175 °C, 350 W for 7 and 10 min, respectively. These new cobalt(II)phthalocyanine complexes were characterized by spectroscopic methods (IR, UV–visible and mass spectroscopy) as well as elemental analysis. Complexes 2 and 6 are employed as catalyst for the oxidation of cyclohexene using tert‐butyl hydroperoxide (TBHP), m‐chloroperoxybenzoic acid (m‐CPBA), aerobic oxygen and hydrogen peroxide (H2O2) as oxidant. It is observed that both complexes can selectively oxidize cyclohexene to give 2‐cyclohexene‐1‐ol as major product, and 2‐cyclohexen‐1‐one and cyclohexene oxide as minor products. TBHP was found to be the best oxidant since minimal destruction of the catalyst, higher selectivity and conversion were observed in the products. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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4.
Firstly, poly[phenyl thiadiazole methacrylamide-co-divinylbenzene-co-2-acrylamido-2-methylpropane sulfonic acid] (PTMAAm-co-DVB-co-AMPS), a new polymer resin was synthesized. This polymer resin was characterized by elemental analyzer, X-ray diffractometer, scanning electron microscope (SEM) and IR spectrometer. The glass column packed with the synthesized polymer resin was used for solid phase extraction (SPE). At the same time, the analytes were separated and preconcentrated from various water, dried vegetables samples and standard reference material (CRM) with SPE and determined by flame atomic absorption spectrometer (FAAS). The experimental conditions of this method such as pH, flow rates of sample, flow rates of eluent, type / concentration / volume of eluent, sample volume and matrix ions were examined. The limits of detection (µg L?1) were calculated (3s) 0.9 for Mn(II), 1.4 for Cd(II), Co(II) and Zn(II), 1.5 for Cr(III), 2.2. for Cu(II), 1.9 for Pb(II),1.5 for Ni(II) and 1.9 for Fe(III) (n = 21). The low relative standard deviation, ≤ 2% (n = 11) and preconcentration factor as 75 for analytes were obtained. 相似文献
5.
Volkan Çakır Dilek Çakır Zekeriya Bıyıklıoğlu Halit Kantekin 《Journal of inclusion phenomena and macrocyclic chemistry》2014,78(1-4):61-70
In this study, a new phthalonitrile derivative 3 bearing 1,3-bis[3(dimethylamino)phenoxy]propan-2-ol 1, metal-free phthalocyanine (Pc) 4, metallophthalocyanines (MPcs) 5–7 and their quaternized derivatives 4a–7a were synthesized. Metal-free Pc 4 was prepared by cyclotetramerization of phthalonitrile derivate 3 and MPcs 5–7 were synthesized by heating 3 with NiCl2, CoCl2 and CuCl2 in n-pentanol in the presence of 1,8-diazabicyclo[5.4.0]undec-7-ene, respectively. Quaternization of the dimethylamino functionality produced quaternized octacationic water soluble metal-free, Ni, Co and Cu Pcs which were soluble in water, DMF, DMSO. The aggregation behaviour of these compounds were investigated in different concentrations of chloroform for metal-free, Ni, Co and Cu Pcs. The effect of solvents on absorption spectra were studied in various organic solvents. The novel compounds were characterized using IR, 1H-, 13C NMR, UV–vis and MS spectral data. 相似文献
6.
Kenan Can Tok Mehmet Gumustas Giorgi Jibuti Halit Sinan Suzen Sibel A. Ozkan Bezhan Chankvetadze 《Molecules (Basel, Switzerland)》2020,25(24)
In a recent study, opposite enantiomer elution order was observed for ketoprofen enantiomers on two amylose-phenylcarbamate-based chiral columns with the same chemical composition of the chiral selector but in one case with coated while in the other with an immobilized chiral selector. In the present study, the influence of this uncommon effect on method validation parameters for the determination of minor enantiomeric impurity in dexketoprofen was studied. The validated methods with two alternative elution orders for enantiomers were applied for the evaluation of enantiomeric impurity in six marketed dexketoprofen formulations from various vendors. In most of these formulations except one the content of enantiomeric impurity exceeded 0.1% (w/w). 相似文献
7.
Preparation of some novel symmetrically tetrasubstituted metal-free phthalocyanine (6) and metallophthalocyanines (7-10) containing four 18-membered tetrathiadiaza macrocycles moieties on peripheral positions has been achieved by cyclotetramerization reaction of phthalonitrile derivative (5) in a multi-step reaction sequence. Metal-free phthalocyanine (6) was synthesized by microwave irradiation of 13,24-bis[(4-methylphenyl)sulfonyl]-6,7,14,15,23,24-hexahydro-13H,22H-tribenzo[b,h,n][1,4,10,13,7,16]tetrathiadiazacyclo-octadecine-18,19-dicarbonitrile (5) in 2-(dimethylamino)ethanol. The metallophthalocyanines (7-10) were prepared by the reaction of the phthalonitrile compound (5) with NiCl2, Zn(CH3COO)2, CoCl2, CuCl2 salts, respectively, by microwave irradiation in 2-(dimethylamino)ethanol for at 175 °C, 350 W. The new compounds were characterized by IR, 1H NMR, 13C NMR, UV-Vis, elemental analysis and MS spectra data. 相似文献
8.
Ümmühan Ocak Miraç Ocak Aysel Başoğlu Semanur Parlayan Dilek Başaran Hakan Alp Halit Kantekin 《Polyhedron》2010
A series of crown ethers carrying an anthracene group with nitrogen–sulfur donor atom, which differ in having three, four and five sulfur atoms in the macrocycle was designed and synthesized by the reaction of the corresponding macrocyclic compound and 9-chloromethyl-anthracene. The influence of metal cations such as Al3+, Zn2+, Fe2+, Fe3+, Co2+, Ni2+, Mn2+, Cu2+, Cd2+, Hg2+ and Pb2+ on the spectroscopic properties of the ligands was investigated in acetonitrile–dichloromethane (1:1) by means of absorption and emission spectrometry. Absorption spectra show isosbestic points in the spectrophotometric titration of Al3+, Zn2+, Fe2+, Fe3+, Cu2+, Hg2+ and Pb2+ the results of which disclosed the complexation compositions and complex stability constants of the novel ligands with these cations. The monoazapentathia crown ether showed sensitivity for Al3+ with linear range and detection limit of 2.6 × 10−6 M–2.6 × 10−5 M and 8.1 × 10−7 M, respectively. 相似文献
9.
Gülsev Dilber Mahmut Durmuş Halit Kantekin Volkan Çakır 《Journal of organometallic chemistry》2011,696(15-16):2805-2814
The synthesis and characterization of peripherally tetra-biphenyl-4-yl-methoxy substituted metal-free (4), Ni(II) (5), Cu(II) (6), Zn(II) (7), Co(II) (8) and Pb(II) (9) phthalocyanine derivatives are reported. These new phthalocyanine derivatives show the enhanced solubility in organic solvents and they have been characterized by a combination of IR, 1H NMR, 13C NMR, UV–vis, mass spectral data, elemental analysis and thermal analysis methods (TG/DTA). The photophysical (fluorescence quantum yield and lifetime) and photochemical (singlet oxygen generation and photodegradation quantum yield) properties of tetra-biphenyl-4-yl-methoxy substituted zinc (II) phthalocyanine derivative (7) are also investigated. The fluorescence of this phthalocyanine derivative (7) is effectively quenched by addition of 1,4-benzoquinone (BQ). 相似文献
10.
We consider a multi-product two-stage production/distribution system design problem (PDSD) where a fixed number of capacitated distribution centers are to be located with respect to capacitated suppliers (plants) and retail locations (customers) while minimizing the total costs in the system. We present a mixed-integer problem formulation that facilitates the development of efficient heuristic procedures. We provide meta-heuristic procedures, including a population-based scatter search with path relinking and trajectory-based local and tabu search, for the solution of the problem. We also develop efficient construction heuristics and transshipment heuristics that are incorporated into the heuristic procedures for the solution of subproblems. We present extensive computational results that show the high performance of the solution approaches. We obtain smaller than 1.0% average optimality gaps with acceptable runtimes, even for relatively large problems. The computational results also demonstrate the effectiveness of the construction and transshipment heuristics that impact the solution quality and overall runtimes. 相似文献