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Öğe Design, preparation and application of a Pirkle-type chiral stationary phase for enantioseparation of some racemic organic acids and molecular dynamics studies(ACG Publications, 2017-11) Çakmak, Reşit; Ercan, Selami; Sünkür, Murat; Yılmaz, Hayrullah; Topal, GirayThis study consists of two parts. In the first part of the study; a Pirkle-type chiral stationary phase was prepared by synthesizing an aromatic amine derivative of (R)-2-amino-1-butanol as a chiral selector and binding to L-tyrosine-modified cyanogen bromide (CNBr)-activated Sepharose 4B and then, packed into the separation column. The chromatographic performance of the separation column was evaluated with racemic mandelic acid and 2-phenylpropionic acid by using phosphate buffers at three different pHs as mobile phase. In the resolution processes, the prepared solutions were loaded onto the separation column at two different concentrations and at three different pHs for each racemic organic acid, separately. Enantiomeric excess (ee%) of the eluates was determined on CHIRALPAK AD-H chiral analytical column by HPLC. The maximum ee% for mandelic acid and 2-phenylpropionic acid was determined to be 60.84 and 27.4, respectively. Separation factors (k1 ’ , k2 ’ , α, and Rs) were calculated for each acid. The structures of the obtained compounds were characterized using the spectroscopic methods (NMR, and elemental analysis). In the second part of the study; enantioselective interactions between the prepared CSP and the analytes have been widely studied by docking, molecular dynamics simulation and quantum mechanical computation methods. The reason of column eluation of rac-2-phenylpropionic acid with lower enantiomeric yield was explained by these techniques.Öğe Mesogenic properties of PAA/6BA binary liquid crystal complexes(Elsevier, 2018-09-19) Okumuş, Mustafa; Eskalen, Hasan; Sünkür, Murat; Özgan , ŞükrüA novel supramolecular liquid crystal complex has been designed and formed from pure liquid crystalspara-azoxyanisole (PAA) and 4-hexylbenzoic acid (6BA). Thermal and microstructural properties offormed PAA/6BA binary liquid crystal complex system are investigated by differential scanning calo-rimeter (DSC), polarized optical microscopy (POM) and X-ray diffractometer (XRD). Fourier transformedinfrared spectroscopy (FTIR) is used to confirm the formation of hydrogen bond between the PAA and6BA molecules. The XRD results show that the molecular ordering of the hydrogen bonded PAA/6BAcomplex is arranged in the orthorhombic structure. The DSC and POM results clearly indicate that thePAA/6BA binary complex exhibits liquid crystalline properties due to the hydrogen bonds formed be-tween the PAA and 6BA molecules. The PAA/6BA complex shows the phase transition peaks indicatingCr/N/I and I/N/SmA/Cr phase sequence during continuous heating and cooling, respectively, byDSC. These phase sequences have also been confirmed by POM observations. Furthermore, the effect ofthe heating rate on the phase transition temperature values is investigated. As the heating rate increases,the phase transition temperature values increase as well. Moreover, the activation energies for the phasetransitions of the PAA/6BA liquid crystal complex are calculated by using Kissinger, Ozawa and Takhormethods. The calculated results clearly show that the phase transitions are regular.Öğe Imine containing C2-Symmetric chiral half sandwich h6-p-cymene-Ru(II)- phosphinite complexes: Investigation of their catalytic activityin the asymmetric transfer hydrogenation of ketones(Journal of Molecular Structure, 2020-01-15) Aral, Tarık; Paşa, Salih; Kayan, Cezmi; Meriç, Nermin; Sünkür, Murat; Aydemir, Murat; Baysal, Akın; Durap, Feyyaz; Saleh, Najmuldain AbdullahNew chiral C2-symmetric bis(phosphinite) ligands containing imine group were synthesized from 1-({[(1R,2R)-2-{[(2-hydroxynaphthalen-1-yl)methylidene] amino}cyclohexyl]- imino}methyl)- naphthalen-2-ol and two equivalents of Ph2PCl, (i-Pr)2PCl or (Cy)2PCl, in high yields. Binuclear C2-symmetric half sandwich η6-p-cymene-Ru(II) complexes of the chiral phosphinite ligands were synthesized by treating of [Ru(η6-p-cymene)(μ-Cl)Cl]2 with the phosphinites in 1:1 M ratio in CH2Cl2. Their catalytic activities in asymmetric transfer hydrogenation (ATH) were investigated for the reaction of acetophenone derivatives with isopropyl alcohol. The corresponding optically active secondary alcohols were obtained in excellent levels of conversion (96–99%) and moderate enantioselectivity (up to 60% ee). Among three complexes investigated, complex 4 was the most efficient one.Öğe Novel C2-symmetric macrocycles bearing diamide-diester groups: Synthesis and enantiomeric recognition for primary alkyl ammonium salts(American Chemical Society, 2008-03-12) Sünkür, Murat; Barış Cebe, Deniz; Hoşgören, Halil; Toğrul, MahmutWe synthesized a series of novel macrocycles with diamide−diester groups (S,S)-1, (S,S)-2, (S,S)-3, and (R,R)-1, derived from dimethyloxalate and amino alcohols by high dilution technique, and evaluated enantiomeric recognition properties of these macrocycles toward primary alkyl ammonium salts by 1H NMR titration. Taking into account the host employed, important differences were observed in the Ka values of (R)-Am and (S)-Am for (S,S)-1 and (R,R)-1 hosts, KS/KR = 5.55 and KR/KS = 3.65, ΔΔGo = 0.43 and −0.32 kJ mol-1, respectively. There seems a general tendency for the host to include the guests with the same absolute configuration.Öğe Synthesis, structural characterization of new macrocyclic Schiff base derived from 1,6-bis(2-formylphenyl)hexane and 2,6-diaminopyridine and its metal complexes(Scientific Publishers, 2008-04) İlhan, Salih; Sünkür, Murat; Temel, Hamdi; Teğin, İbrahimA macrocyclic ligand has been synthesized by reaction of 2,6-diaminopyridine and 1,6-bis(2-formylphenyl).hexane. Its complexes with Cu(II), Ni(II), Pb(II), Zn(II), Cd(II) and La(III) have been synthesized by the reaction of ligand and Cu(ClO4)(2)center dot 6H(2)O, Ni(ClO4)(2)center dot 6H(2)O, Pb(ClO4)(2)center dot 6H(2)O, Zn(ClO4)(2)center dot 6H(2)O, Cd(ClO4)(2)center dot 6H(2)O and La(ClO4)(3)center dot 6H(2)O, respectively. The ligand and its metal complexes have been characterized. All complexes are diamagnetic while the Cu(II) complex is binuclear.
