Search

Your search keyword '"Gök, Halil Zeki"' showing total 46 results
Start Over Author "Gök, Halil Zeki"
46 results on '"Gök, Halil Zeki"'

2. A Novel Mesoporous SBA‐15 Supported Bifunctional Heterogeneous Catalyst for Base‐Free Transfer Hydrogenation Reaction of Ketones.

Author

Gök, Halil Zeki, Arlı, Osman Tayyar, and Gök, Yaşar

Subjects
*TRANSFER hydrogenation, *HETEROGENEOUS catalysis, *HETEROGENEOUS catalysts, *CATALYTIC hydrogenation, *MESOPOROUS silica
Abstract

ABSTRACT Among the problems encountered in the catalytic transfer hydrogenation reactions of ketones, the base sensitivity of ketones and the corrosive effects of the bases used in the reaction have an important place especially in industrial terms. Although there are various approaches to overcome this problem, solutions based on the intrinsic properties of the catalyst used seem more suitable. Within the scope of this study, a novel heterogeneous catalyst was prepared for the transfer hydrogenation reaction of ketones, which can operate in base‐free environment. To prepare the heterogeneous catalyst, 1,2‐diphenylethane‐1,2‐diamine was first tosylated and then the silyl derivative was synthesized and grafted onto mesoporous silica SBA‐15. Characterizations of the obtained heterogeneous catalyst and SBA‐15 were carried out by X‐ray diffractometer (XRD), N2 sorption, thermogravimetric analysis (TGA), scanning electron microscope (SEM), energy dispersive X‐ray analysis, and Fourier transform infrared (FT‐IR) analysis. The results obtained showed that the functionalized 1,2‐diphenylethane‐1,2‐diamine compound was successfully immobilized into the SBA‐15 structure. Determination of the catalytic activity of the heterogeneous catalyst was carried out in transfer hydrogenation reactions of various aromatic ketones. After determining the optimum reaction conditions with acetophenone, a conversion rate of (70%) was observed in the acetophenone to 1‐phenylethanol reaction that took place without a base. Under same conditions a higher conversion rate of (73%) was observed in the 4′‐chloroacetophenone to 1‐(4‐chlorophenyl)ethanol reaction. In the reactions performed to determine recyclability, after a 70% conversion rate, 61% and 65% conversion rates, respectively, were observed in the reaction from acetophenone to 1‐phenylethanol under the same conditions. [ABSTRACT FROM AUTHOR]

Published
2024
Full Text
View/download PDF

3. Piperazindion Birimi İçeren Yeni Bir Ftalosiyanin Bileşiğinin Sentezi, Karakterizasyonu ve Metal Ekstraksiyon Özelliklerinin İncelenmesi.

Author

GÖK, Halil Zeki

Subjects
MACROCYCLIC compounds, LIQUID-liquid extraction, PHTHALOCYANINE derivatives, METAL ions, TRANSITION metals, BENZENEDICARBONITRILE
Abstract

Copyright of Afyon Kocatepe University Journal of Science & Engineering / Afyon Kocatepe Üniversitesi Fen Ve Mühendislik Bilimleri Dergisi is the property of Afyon Kocatepe University, Faculty of Science & Literature and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Published
2024
Full Text
View/download PDF

12. Preparation of mesoporous silica and organosilica nanostructures functionalized with C2‐symmetric diol and their catalytic performance in diethylzinc addition to aromatic aldehydes.

Author

Gök, Yaşar and Gök, Halil Zeki

Subjects
*MESOPOROUS silica, *AROMATIC aldehydes, *HETEROGENEOUS catalysis, *HOMOGENEOUS catalysis, *CATALYTIC activity, *HETEROGENEOUS catalysts
Abstract

In this study, heterogenization of C2‐symmetric (1R,2R)‐1,2‐bis(4‐(3‐(triethoxysilyl)propyl)phenyl)ethane‐1,2‐diol compound and investigation of the effect of structural arrangements of nanocatalysts on catalytic activity were carried out. For this, bissilyl derivative of (1R,2R)‐1,2‐bis(4′‐bromophenyl)‐ethane‐1,2‐diol, named as C2‐BSi, was obtained by 2‐step synthesis. Then, mesoporous silica nanocatalysts C2‐BSi@SBA‐15 and C2‐BSi@MCM‐41 were synthesized by grafting of C2‐BSi onto SBA‐15 and MCM‐41, whereas mesoporous organosilica nanocatalysts C2‐BSi‐MON‐(a) and C2‐BSi‐MON‐(b) were synthesized by co‐condenzation of C2‐BSi and tetraethyl orthosilicate (TEOS). Structure determinations of synthesized organic substances were performed by 1H, 13C NMR, Fourier transform infrared (FT‐IR), polarimeter, and mass analysis, whereas the structural properties of heterogeneous catalysts C2‐BSi@SBA‐15, C2‐BSi@MCM‐41, C2‐BSi‐MON‐(a), and C2‐BSi‐MON‐(b) were determined by FT‐IR, X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), and N2 sorption analyses. The catalytic activities of novel heterogenous materials were tested in the reaction of Ti‐promoted enantioselective diethylzinc addition to aromatic aldehydes. The effects of the structural arrangements of the prepared heterogeneous catalyst on the catalytic activity were examined and compared with the catalytic activity values of their homogeneous analog. According to the results, all catalysts catalyzed the reactions and afforded the corresponding products with high conversion (82–99%) but low enantioselectivity (rac‐7% ee). The conversion values in heterogeneous catalysis were higher than those in homogeneous catalysis. C2‐BSi‐MON‐(a) with the largest pore width stood out as the most effective catalyst (99% conversion, 7% ee). The findings from the catalytic activity experiments confirmed that the structural arrangement of the nanocatalysts has an effect on the performance of the catalysts in the reaction. [ABSTRACT FROM AUTHOR]

Published
2024
Full Text
View/download PDF

23. Preparation of Mesoporous Silica Nanostructure Functionalized With Hydrobenzoin Substituted Phthalocyanine and Its Catalytic Performance in Benzyl Alcohol Oxidation.

Author

Gök, Yaşar, Arlı, Osman Tayyar, Gök, Halil Zeki, and Erdem, Recep

Subjects
*BENZYL alcohol, *MESOPOROUS silica, *HETEROGENEOUS catalysis, *CATALYTIC activity, *HETEROGENEOUS catalysts, *BENZALDEHYDE, *ALCOHOL oxidation
Abstract

ABSTRACT In this study, a new mesoporous silica nanostructure functionalized with hydrobenzoin substituted cobalt (II) phthalocyanine (MCM‐41‐CoPc) was prepared by grafting first 3‐chloropropyltriethoxysilane (CPTES) and then peripherally hydrobenzoin substituted cobalt (II) phthalocyanine (CoPc) onto mesoporous silica nanomaterial (MCM‐41). The structural properties of heterogeneous catalyst MCM‐41‐CoPc were elucidated by FT‐IR, XRD, TEM, EDS, TGA, solid‐state UV–Vis and N2 sorption analyses. The catalytic performance of MCM‐41‐CoPc was investigated in the oxidation of benzyl alcohol to benzaldehyde. To find the best catalytic conditions for aldehyde selectivity, the effect of the different parameters such as temperature, reaction time, oxidant, solvent, amount of the substrate, and oxidant on the catalytic activity of MCM‐41‐CoPc was investigated in detail. The selective oxidation of benzyl alcohol to benzaldehyde in the presence of MCM‐41‐CoPc was achieved with high aldehyde selectivity (98%) and moderate conversion (57%). The reusability of MCM‐41‐CoPc was tested in three consecutive cycle and no catalytic activity loss was observed. Additionally, it has been determined that the product selectivity can be controlled depending on the type of reaction solvent. When ethyl acetate was used as the solvent, 98.5% conversion rate and 96% benzoic acid selectivity were obtained. [ABSTRACT FROM AUTHOR]

Published
2024
Full Text
View/download PDF

24. A novel n-pivot macrocyclic ligand and its Cobalt(II) phthalocyanine derivative: synthesis, characterization and extractant properties

Author

GÖK, Halil Zeki and GÖK, Yaşar

Subjects
Engineering, Mühendislik, Phthalocyanine,Macrocycle,N-Pivot,Transition metal,Solvent extraction
Abstract

In thisstudy, the synthesis of a novel N-pivot 12-membered macrocyclic ligand withmixed donor atoms 2, which is aphthalonitrile derivative, and a new cobalt(II) phthalocyanine complex 3 obtained by cyclotetramerizationreaction of 2 were described. Newly synthesizedcompounds were characterized by using several spectroscopic techniques such asIR, UV-Vis, 1H and 13C NMR, MS and elemental analysis.These macrocyclic systems 2 and 3 were investigated as extractants inliquid-liquid extraction technique to reveal metal ion binding capabilitytowards transition metals such as Ag(I), Hg(II), Cd(II), Zn(II), Cu(II),Ni(II), Pb(II) and Co(II). The highestextractability from aqueous phase to organic phase was found for Hg(II) cationover the other metal cations with cobalt(II) phthalocyanine 3. The extraction percentage of Hg(II)cation from aqueous phase to chloroform in the presence of cobalt(II)phthalocyanine 3 as extractant wasfound as 96.0%.

Published
2018

26. Oxidation of benzyl alcohol by novel peripherally and non‐peripherally modular C2‐symmetric diol substituted cobalt (II) phthalocyanines.

Author

Gök, Halil Zeki, Gök, Yaşar, and Yılmaz, Mustafa Kemal

Subjects
*BENZYL alcohol, *COBALT, *ALCOHOL oxidation, *GLYCOLS, *BENZENEDICARBONITRILE, *PHENYL group, *MODULAR construction, *CATALYSTS
Abstract

In this study, a modular ligand structure was designed by altering the binding position of the phenyl group at backbone of hydrobenzoin. A series of regio isomeric substituted phthalonitriles derived from this modular C2‐symmetric ligand was synthesized and characterized. Then, eight cobalt (II) phthalocyanines (CoPc) were obtained from the reaction of phthalonitrile derivatives with cobalt (II) chloride. The catalytic activities of synthesized cobalt (II) phthalocyanines were tested for benzyl alcohol oxidation in acetonitrile using tert‐butylhydroperoxide as the oxygen source and in the presence of N‐bromosuccinimide as an additive at 80 °C for 5 hr of the reaction. In this sense, the effect of substrate to catalyst ratio and oxidant to catalyst ratio have been studied in detail for getting the highest benzaldehyde selectivity (up to 83%). The effect of structural design of substituents at peripheral or non‐peripheral positions of phthalocyanine skeleton on the catalytic activity performance of cobalt (II) phthalocyanines in benzyl alcohol oxidation was also clarified. All newly synthesized compounds are characterized by FT‐IR, 1H NMR, IR, UV–Vis and MALDI‐TOF MS spectral data. [ABSTRACT FROM AUTHOR]

Published
2020
Full Text
View/download PDF

29. Peripherally 1,2-dinaphthyl ethanediol substituted phthalocyanine complexes: synthesis, characterization, aggregation, and application in benzyl alcohol oxidation at room temperature.

Author

GÖK, Halil Zeki and YILMAZ, Mustafa Kemal

Subjects
*BENZYL alcohol, *ALCOHOL oxidation, *ETHYLENE glycol, *BENZENEDICARBONITRILE, *PHTHALOCYANINE derivatives, *BENZALDEHYDE, *CATALYTIC activity, *COBALT
Abstract

In this study, the synthesis of a novel 1,2-dinaphthyl ethanediol substituted phthalonitrile (2) together with tetra-substituted zinc(II) phthalocyanine (Pc) (3) and cobalt(II) Pc (4) bearing 1,2-dinaphthyl ethanediol at peripheral positions was described. The aggregation behaviors of metallophthalocyanines 3 and 4 in solution were investigated by carrying out Beer-Lambert experiments at different concentrations. In addition, the catalytic activity of new cobalt(II) Pc 4 was investigated for benzyl alcohol oxidation. Benzyl alcohol was converted to benzaldehyde using cobalt(II) Pc 4 as a catalyst by a conversion of 99% with selectivity of 100% at room temperature in 1 h. Several spectroscopic techniques such as FT-IR, UV-Vis, 1 H and 13 C NMR, and MALDI-TOF MS were used for the characterization of the newly synthesized compounds. [ABSTRACT FROM AUTHOR]

Published
2019
Full Text
View/download PDF

31. Peripherally 1,2-dinaphthyl ethanediol substituted phthalocyanine complexes: synthesis, characterization, aggregation, and application in benzyl alcohol oxidation at room temperature

Author

GÖK, Halil Zeki and YILMAZ, Mustafa Kemal

Subjects
Engineering, Metallophthalocyanine,catalysis,$C_{2}$-symmetric,benzyl alcohol oxidation,aggregation, Mühendislik
Abstract

In this study, the synthesis of a novel 1,2-dinaphthyl ethanediol substituted phthalonitrile (2) together with tetra-substituted zinc(II) phthalocyanine (Pc) (3) and cobalt(II) Pc (4) bearing 1,2-dinaphthyl ethanediol at peripheral positions was described. The aggregation behaviors of metallophthalocyanines 3and 4 in solution were investigated by carrying out Beer-Lambert experiments at different concentrations. In addition, the catalytic activity of new cobalt(II) Pc 4 was investigated for benzyl alcohol oxidation. Benzyl alcohol was converted to benzaldehyde using cobalt(II) Pc 4 as a catalyst by a conversion of 99% with selectivity of 100% at room temperature in 1 h. Several spectroscopic techniques such as FT-IR, UV-Vis, $^{1}$H and $^{13}$C NMR, and MALDI-TOF MS were used for the characterization of the newly synthesized compounds.

Published
2014

33. Synthesis of C2-Symmetric Bisphosphines and Their Application in Enantioselective Transition Metal Catalysis.

Author

Gök, Halil Zeki, Kılıçarslan, Seda, and Gök, Yaşar

Subjects
*ENANTIOSELECTIVE catalysis, *CHEMICAL synthesis, *HYDROGENATION, *RUTHENIUM, *CHEMICAL reactions
Abstract

C2-symmetric bisphosphine ligands (with a dioxolane backbone) have been synthesized by using corresponding chiral bromosubstituted hydrobenzoin derivatives in two steps with moderate yields. The last step for desired bisphosphines defined the electronic and steric properties of the chelating atoms by the treatment of aryl or alkyl substituted chlorophosphine compounds in the presence of a base. These synthesized ligands have been evaluated in different catalytic reactions. The first application has been the palladiumcatalyzed enantioselective allylic alkylation which is regarded as a remarkable reaction for forming enantioselective carbon-carbon bond (up to 63 % ee and 98 % chemical yield). The ruthenium-catalyzed enantioselective transfer hydrogenation reaction has been the second application for the evaluating of the catalysts (up to > 99 % conversion with no enantioselectivity). [ABSTRACT FROM AUTHOR]

Published
2018
Full Text
View/download PDF

35. Karışık donörlü makrosiklik grup içeren yeni ftalosiyanin sentezi ve özelliklerinin incelenmesi

Author

Gök, Halil Zeki, Kantekin, Halit, and Kimya Anabilim Dalı

Subjects
Chemistry, Kimya
Abstract

Bu çalışmada, N2S5O2 ve N2S7 tipi donör atomları içeren yeni 27-üyeli makrosiklerinsentezi ve bunların metalsiz ve metalli ftalosiyanin türevleri sentezlenmiştir. Bu amaç için,1,2-bis (2â²-aminofenilsulfaniletoksi)-4,5-dibromobenzen ile klorasetil klorüründiklorometan içerisinde 0-5 0C'deki reaksiyonundan elde edilen (1) bileşiği, 2,2â²-ditiyoetantiyol ile reaksiyona sokularak bisamid makrosiklik (2) bileşiği elde edildi.ndirgenmiş makrosiklik bileşiği (3), (2) bileşiğinin sodyum borhidrür-bor trifluorür etileter kompleksi ile kuru THF içerisinde indirgenmesi ile elde edildi. Dibromo türevleri (2)ve (3), DMF içerisinde üç ekivalent CuCN ile reaksiyounundan (4) ve (8) elde edildi. 1,2-Bis(2-iyodoetilmerkapto)-4,5-disiyanobenzen ile 2-aminotiyofenol'ün kuru Na2CO3 içerenTHF içerisinde argon atmosferindeki reaksiyonu ile (11) bileşiği elde edildi. Daha sonra,(11) bileşiğinin kloroasetil klorür ile diklorometan içerisinde reaksiyonundan elde edilen(12) bileşiği, 2,2â²-ditiyoetantiyolün DMF içerisindeki çözeltilerinin, kuru Na2CO3 içerenDMF çözeltisi içerisine eş zamanlı ilavesi yapılarak ftalonitril türevi (13) bileşiği eldeedildi. Ftalonitril türevlerinin (4), (8) ve (13), kuru 2-(dimetilamino)etanol ile 24 saat gerisoğutucu altında kaynatılması ile gerçekleştirilen siklotetramerizasyon reaksiyonu sonucumetalsiz ftalosiyan bileşikleri (5), (9) ve (14) elde edildi. Nikel(II) ftalosiyanin bileşikleri(6) ve (10), (4) ve (8) bileşiklerinin susuz NiCl2 ile kuru kinolin içerisindekireaksiyonundan elde edildi. Ftalonitril bileşiklerinin (4) ve (13), kinolin, susuzZn(CH3CO)2 ile argon atmosferi altında kaynatılması reaksiyonu sonucu, sırası ileçinko(II) ftalosiyanin bileşikleri (7) ve (15) elde edildi. Elde edilen yeni bileşiklerinyapıları, elementel analiz, 1H NMR, 13C NMR, IR, UV-Vis ve kütle spektral verilerikullanılarak karakterize edilmiştir. In this work, new 27-membered macrocyclic compounds containing both N2S5O2 andN2S7 type donor atoms and their metal-free and metallophthalocyanines derivatives weresynthesized. For this purpose, the synthesis of bisamide macrocyclic (2) was performed bythe reaction of 2,2â²-dithioethanthiol with the compound (1) obtained from the reaction of1,2-bis (2â²-aminophenylsulfanylethoxy)-4,5-dibromobenzene with chloroacetic anhydridein dichloromethane. The reduced macrocyclic compund (3) was obtained from theprecursor (2) by using sodium boronhydride-boron trifluoride ethyl etherate in dry THF at0-5 0C under argon atmosphere. The dibromo derivatives (2) and (3) were converted intodicyano derivatives (4) and (8) by refluxing in dry DMF with three equivalents of CuCN.1,2-Bis(2-iodoethylmercapto)-4,5-dicyanobenzene was converted to compound (11). Lateron, the synthesis of the macrocycle (13) was performed by a reaction of 2,2â²-dithioethanthiol with (12) in DMF containing anhydrous Na2CO3 by the following areaction of (11) with chloroacetic anhydride in dichloromethane, affording the compound(12). The cyclotetramerization of the phthalonitrile derivatives (4), (8) and (13) to themetal-free phthalocyanines (5), (9) and (14), respectively, were accomplished in dry 2-(dimethylamino)ethanol. Ni(II) phthalocyanines (6) and (10) were synthesized by thereaction of (4) and (8) with anhydrous NiCl2 in dry quinoline, respectively. Thepreparation of Zn(II) phthalocyanines (7) and (15) from the dicyano compounds (4) and(13) with anhydrous Zn(CH3CO)2, respectively, were carried out in quinoline at refluxtemperature for 8 h and 7 h. The new compounds were characterized by a combination ofelemental analysis and 1H NMR, 13C NMR, IR, UV-Vis and MS spectral data. 243

Published
2006

41. Enantioselective Ethylation of Various Aldehydes Catalyzed by Readily Accessible Chiral Diols.

Author

Gök, Yaşar, Kiliçarslan, Seda, Gök, Halil Zeki, and Karayiğit, İlker Ümit

Subjects
CHIRALITY, GLYCOLS, CATALYSIS, ENANTIOMERS, ALDEHYDES
Abstract

Four chiral C2-symmetric diols were synthesized in a straightforward three-step reaction and demonstrated excellent and good overall yields. Their catalytic activities were examined via the addition of diethylzinc to various aldehydes. The of diethylzinc to 2-methoxybenzaldehyde gave the corresponding chiral secondary alcohol with high yields (up to 95%) and moderate to good enantiomeric excess (up to 88%). All synthesized ligands were evaluated in the addition of diethylzinc to various aldehydes in the presence of an additional metal such as Ti(IV) complexes. Chirality 28:593-598, 2016. © 2016 Wiley Periodicals, Inc. [ABSTRACT FROM AUTHOR]

Published
2016
Full Text
View/download PDF

42. Periferal 1,2-di(1-naftil)-1,2-etandiol substitue ftalosiyaninlerin sentezi, karakterizasyonu ve agregasyon özelliklerinin incelenmesi

Author

Başay, Ayhan, Gök, Halil Zeki, and Kimya Anabilim Dalı

Subjects
Chemistry, Kimya
Abstract

1,2-dinaftil ethandiol substitute ftalonitril 2 ve peripheral konumlarda 1,2-dinaftil etandiol'ün substitue edildiği tetra-substitue çinko(II) ftalosiyanin ve kobalt(II) ftalosiyanin bileşiklerinin sentezi ve karakterizasyonu bu çalışma kapsamında yapılmıştır. Ftalosiyanin bileşiklerinin agregasyon özellikleri üzerine çözücü türünün ve ftalosiyanin derişiminin etkisi incelenmiştir. Ftalosiyanin bileşiklerinin agregasyon özelliklerini incelemek için, ftalosiyanin bileşiklerinin THF ve DMF içerisinde 10 x 10-6 ve 2 x 10-6 mol dm-3 derişimine sahip çözeltileri ile Beer-Lambert deneyi yapılmıştır. Ftalosiyanin kompleksleri3 ve 4 çalışılan 10 x 10-6 ve 2 x 10-6 mol dm-3 derişim aralığında THF ve DMF çözücüleri içerisinde agregasyon eğilimi göstermemişlerdir. Yeni sentezlenen bileşiklerin yapısal tayini 1H NMR, IR, UV-Vis and MALDI-TOF MS spectral verileri kullanılarak yapılmıştır. The synthesis and characterization of a novel 1,2-dinaphthyl ethanediol substituted phthalonitrile 2 together with tetra-substituted zinc(II) phthalocyanine 3 and cobalt(II) phthalocyanine 4 bearing 1,2-di(naphthalen-1-yl)ethane-1,2-diol at peripheral positions were described. The solvent and concentration effects on the aggregation properties of the phthalocyanines were determined. To investigate the aggregation behaviors of phthalocyanine complexes 3 and 4, Beer-Lambert's experiment was carried out at the concentrations between 10 x 10-6 and 2 x 10-6 mol dm-3 in THF and DMF. The phthalocyanine complexes 3 and 4 demonstrated no aggregation behavior in DMF and THF from concentrations between 10 x 10-6 and 2 x 10-6 mol dm-3. The structures of the newly synthesized compounds are characterized by 1H NMR, IR, UV-Vis and MALDI-TOF MS spectral data. 82

Published
2018

43. Periferal ve non-periferal hidrobenzoin substitue optikçe aktif ftalosiyaninlerin sentezi, karakterizasyonu ve agregasyon özelliklerinin incelenmesi

Author

Kiliç, Yunus, Gök, Halil Zeki, and Kimya Anabilim Dalı

Subjects
Chemistry, Kimya
Abstract

Periferal ve non-periferal konumlarda dört kiral hidrobenzoinin bağlı olduğu optikçe aktif yeni dörtmetalo ftalosiyanin (Zn ve Co) bileşiklerinin sentezi ve karakterizasyonu bu çalışma kapsamında yapılmıştır. Sentezlenen bileşiklerin yapısal karakterizasyonu1H NMR, IR, UV-Vis, Dairesel dikroizm (CD) ve MALDI-TOF MS spektral verileri kullanılarak yapılmıştır. Sentezlenen tüm ftalosiyanin kompleksleri yaygın olarak kullanılan organik çözücüler içerisinde oldukça yüksek çözünürlüğe sahiptir. Periferal ve non-periferal konumlarda hidrobenzoin içeren tetra-substitue metalo ftalosiyanin bileşiklerinin spektral ve agregasyon özellikleri kıyaslamalı olarak çalışılmıştır. Ftalosiyanin kompleksleri 4-7 çalışılan 2-10x10-6 mol dm-3konsantrasyon aralığında tetrahidrofuran ve N,N-dimetilformamid içerisinde agregasyon eğilimi göstermemişlerdir The synthesis and characterization of a novel hydrobenzoin substituted optically active phthalonitrile 2and 3 together with optically active tetra-substituted zinc(II) phthalocyanine 4 and 6, and cobalt(II) phthalocyanine 5 and 7bearing hydrobenzoinat peripheral and non-peripheral positions, respectively, were described. Structures of the newly synthesized compounds are determined by 1H NMR, UV-Vis, Circular Dichroism (CD), IR and mass spectral data. The solvent and concentration effects on the aggregation properties of the phthalocyanines were determined. To investigate the aggregation behaviors of phthalocyanine complexes 4-7, Beer-Lambert's experiment was carried out at the concentrations between 10x10-6 and 2x10-6 mol dm-3 in tetrahydrofuran and N,N-dimethylformamide. The phthalocyanine complexes 4-7 demonstrated no aggregation behavior in N,N-dimethylformamide and tetrahydrofuran from concentrations in the range of 2-10x10-6 mol dm-3. 94

Published
2018

44. Yeni bir makrobisiklik bileşiğin sentezi ve metal iyon bağlama özelliklerinin incelenmesi

Author

Eker, Esra, Gök, Halil Zeki, and Kimya Anabilim Dalı

Subjects
Chemistry, Kimya
Abstract

Bu tez çalışmasında, yeni bir makrosbisiklik ligandın sentezi, karakterizasyonu ve metal iyon bağlama özellikleri çalışılmıştır. Elde edilen yeni bileşiklerin yapıları, elementel analiz, 1H NMR, 13CNMR, IR ve kütle spektral verileri kullanılarak karakterize edilmiştir. Yeni makrobisiklik ligandın seçilen metal katyonlarına karşı ekstraksiyon etkinliğini incelemek için çözücü ekstraksiyon deneyleri gerçekleştirilmiştir. Ekstraksiyon etkinliklerini belirleyebilmek için diklorometan ve kloroform organik çözücüleri kullanılmıştır. Ağır ve değerli metallerin seçimli ekstraksiyonu, bunların ticari değerleri ve zehirli etkilerinden dolayı oldukça önemlidir. Yapılan deneysel çalışmalarda, makrosiklik ligand (8), Ag+ ve Hg2+ katyonlarını oldukça etkili ve seçimli bir şekilde ekstrakte ederken, (9) ve (10) bileşikleri Ag+ ve Hg2+ katyonlarını daha düşük seçimlilikle iyi ekstrakte edebildiği gözlenmiştir. Çalışılan ligandlar arasında her iki organik çözücü içerisine en yüksek Ag+ ekstraksiyonu makrobisiklik ligand (10) için gözlenmiştir. Makrobisiklik ligand (10), Ag+ iyonunu diklorometan fazına %96,7 ve kloroform fazına %96,9 gibi oldukça dikkat çeken değerler ile ekstrakte etmiştir. This study describes the synthesis, structural characterization of a new macrobicyclic ligand and its use in metal cation extraction. The structures of new compounds were characterized by a combination of elemental analysis and 1H NMR, 13C NMR, IR and MS spectral data. Solvent extraction experiments were performed in order to determine the extraction behavior of new macrobicyclic ligand towards selected metal cations. Two different organic solvents, dichloromethane and chloroform, were tested to reveal extraction efficiency. Selective extraction of heavy metals and precious metal is highly demanded due to their toxicity and commercial importance. From the experimental results, macrocyclic ligand (8) is very effective and selective for Ag+ and Hg2+ cations, whereas compounds (9) and (10) show good extraction behavior without selectivity towards Ag+cation. The highest Ag+ extraction behavior among the tested ligands in both organic solvents was observed for macrobicyclic ligand (10). Macrobicycle (10) demonstrated remarkable affinity towards the Ag+ ion by 96.7% and 96.9% to the dichloromethane and chloroform phase, respectively. 75

Published
2015

45. Karışık donörlü makrosiklik grup ihtiva eden yeni bir ftalosiyanin sentezi ve metal iyon bağlama özelliklerinin incelenmesi

Author

Doğan, Özgür, Gök, Halil Zeki, and Kimya Anabilim Dalı

Subjects
Chemistry, Kimya
Abstract

Bu çalışma, 18 üyeli karışık donörlü makrosikliklerin periferal olarak bağlı olduğu metalsiz ftalosiyanin ve metalli ftalosiyaninlerin sentezini bildirmektedir. Makrosiklik ligand ve ftalosiyanin türevlerinin spektroskopik ve metal iyon bağlama özellikleri incelenmiştir. Bu amaç için, metalsiz ftalosiyanin ve metalli ftalosiyanin bileşiklerinin elektronik absorpsiyon spektrumları DMF ve THF içerisinde alınmıştır. Ag(I), Hg(II), Cd(II), Zn(II), Cu(II), Ni(II), Pb(II) ve Co(II) gibi metal pikratlarının sulu fazdan organik faza taşınımı, makrosiklik ligand ve metalli ftalosiyanin bileşikleri kullanılarak sıvı sıvı ekstraksiyonu yöntemi ile çalışılmıştır. Elde edilen yeni bileşiklerin yapıları, elementel analiz, 1H NMR, 13C NMR, IR, UV-Vis ve kütle spektral verileri kullanılarak karakterize edilmiştir. This study describes the synthesis of a metal-free phthalocyanine and metallophthalocyanines peripherally substituted by macrocycles of 18-membered with mixed donor atom sets. The spectroscopic and metal ion binding properties of macrocyclic ligand and its phthalocyanine derivatives have been examined. For these purposes, electronic absorption properties for metal-free phthalocyanines and metallophthalocyanines were studied in dimethylformamide and tetrahydrofuran. The liquid-liquid extraction of metal picrates such as Ag(I), Hg(II), Cd(II), Zn(II), Cu(II), Ni(II), Pb(II) and Co(II) from aqueous phase to the organic phase was carried out using macrocyclic ligand and metallophthalocyanines. All new compounds were characterized by a combination of elemental analysis and 1H NMR, 13C NMR, IR, UV-Vis and MS spectral data. 97

Published
2015

46. Karışık donörlü makrosiklik grup ihtiva eden yeni bir ftalosiyanin sentezi ve elektrokimyasal karakterizasyonu

Author

Farsak, Berna, Gök, Halil Zeki, and Kimya Anabilim Dalı

Subjects
Chemistry, Kimya
Abstract

Bu çalışmada, ilk olarak bir bisamid bileşiği (2) ve N2S4O tipi donör atomları içeren yeni 21-üyeli makrosiklik bileşiği (3) sentezlenmiştir. Çevresel konumlarda 21-üyeli oksatetratiyadiaza makrosiklik bileşiğini ihtiva eden metalsiz, Zn(II) ve Co(II) metalloftalosiyaninler, makrosiklik bileşiğin (3) siklotetramerizasyon tepkimesi sonucunda elde edilmişlerdir. Bu ftalosiyanin bileşiklerinin agregasyon özellikleri üzerine derişim etkisi çalışılmıştır. Metalsiz ve metalloftalosiyaninler, DMF içerisinde 10 x 10^-6 ve 1 x 10^-6 mol dm^-3 derişim aralığında agregasyon eğilimi göstermemişledir. Ftalosiyaninlerin agregasyon özellikleri DMF, THF ve CH2Cl2 gibi farklı çözücüler içerisinde de incelenmiştir. Elde edilen yeni bileşiklerin yapıları, elementel analiz, 1H NMR, 13C NMR, IR, UV-Vis ve kütle spektral verileri kullanılarak karakterize edilmiştir. Ftalosiyanin bileşiklerinin elektrokimyasal karekterizasyonu dönüşümlü voltametri tekniği kullanılarak incelenmiştir.Anahtar kelimeler: Makrosiklik Bileşik, Ftalosiyanin, Dönüşümlü Voltametri In this study, a bisamide compound (2) and a novel 21-membered macrocycle (3) containing N2S4O donor atoms were synthesized as first. The syntheses of novel metal-free, Zn(II) and Co(II) phthalocyanines containing four 21-membered oxatetrathiadiaza macrocycles on peripheral positions were prepared by cyclotetramerization of a novel macrocyclic compound (3). Concentration effect on the aggregation properties of those phthalocyanines was investigated. There was no aggregation behaviour in DMF for the metal-free and metallophthalocyanine complexes from concentration between 10 x 10^-6 and 1 x 10^-6 mol dm^-3. The aggregation properties of all phthalocyanines were also investigated in different solvents such as DMF, THF and CH2Cl2. All new compounds were characterized by a combination of elemental analysis and 1H NMR, 13C NMR, IR, UV-Vis and MS spectral data, all of which were in agreement with the proposed structures. Electrochemical characterization of phthalocyanines was investigated by using the technique of cyclic voltammetry. Key Words: Macrocyclic Compound, Phthalocyanine, Cyclic Voltammetry 109

Published
2012

Catalog

Books, media, physical & digital resources
See catalog results