BAZI s-TRİAZİN KÖPRÜLÜ KALİKSAREN KOMPLEKSLERİNİN SENTEZİ VE KARAKTERİZASYONU
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2021-07-12
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info:eu-repo/semantics/openAccess
Özet
Bu çalışmada siyanürik klorür 0 °C’da ayrı ayrı 2,4-dihidroksibenzaldehit, 3,5-dihidroksibenzilalkol ve metil-3,5-dihidroksibenzoat ile reaksiyona tabi tutularak 2,4-bis((4,6-dikloro-1,3,5-triazin-2-il)oksi)benzaldehit, (3,5-bis((4,6-dikloro-1,3,5-triazin -2-il)oksi)fenil)metanol ve metil-3,5-bis((4,6-dikloro-1,3,5-triazin-2-il)oksi)benzoat elde edildi. Daha sonra bu elde edilen bileşikler 28 °C’da sırasıyla tekrar 2,4-dihidrok-sibenzaldehit, 3,5-dihidroksibenzilalkol ve metil-3,5-dihidroksibenzoat ile reaksiyona tabi tutularak ID1, ID3 ve ID6 olarak kodladığımız ara s-triazin köprülü kaliksaren bileşikleri elde edildi. ID1 kodlu bileşiğin iki kez 1:2 mol oranında 4-aminobenzoik asit ile reaksiyonundan ID2 olarak kodladığımız ilk s-triazin köprülü kaliksaren ligandımız elde edilmiştir. ID3 kodlu ara ürünün 1:2 mol oranında 4-aminobenzoik asit ile reaksiyonundan ID4 kodlu ligand, 1:2 mol oranında 4-hidroksibenzoik asit ile reaksiyonundan ID5 kodlu ligand elde edilmiştir. ID6 kodlu ara ürünün 1:2 mol oranında 4-aminobenzoik asit ile reaksiyonundan ID7 kodlu ligand, 1:2 mol oranında 4-hidroksibenzoik asit ile reaksiyonundan ID8 kodlu ligand elde edilmiştir. Elde edilen bu ID2, ID4, ID5, ID7 ve ID9 kodlu ligandların her biri uygun mol oranında 1,4-diok-san ortamında [(MSalen/Saloph)2O] (M=Cr3+, Fe3+ ve Co3+) başlangıç kompleksleri ile reaksiyonundan (MSalen/Saloph) şapkalı s-triazin köprülü kaliksaren kompleks-leri elde edilmiştir. Elde edilen bu ligandlar 1H-NMR (DMSO-d6), FT-IR spektroskopisi ve elementel analiz yöntemleri ile karakterize edilmiştir. Kompleksler ise FT-IR, UV-Vis spektroskopisi, elementel analiz, manyetik süssebtibilite ve TGA-DTA teknikleri kullanılarak karakterize edilmiştir. Komplekslerdeki metal miktarları ise ICP-AES spektroskopisi ile belirlenmiştir.
In this study, 2,4-bis((4,6-dichloro-1,3,5-triazin-2-yl)oxy)benzaldehyde, (3,5-bis((4,6-dichloro-1,3,5-triazin-2-yl)oxy)phenyl)methanol and methyl-3,5-bis((4,6-dichloro-1,3,5-triazin-2-yl)oxy)benzoate compounds were obtained by reacting, separately, cyanuric chloride with 2,4-dihydroxybenzaldehyde, 3,5-dihydroxybenzyl alcohol and methyl-3,5-dihydroxybenzoate at 0 °C. Then, s-triazine bridged calixarens codded as ID1, ID3 and ID6 were obtained by reacting the compounds with 2,4-dihydroxybenzaldehide, 3,5-dihydroxybenzylalcohol and methyl-3,5-dihydroxybenzoate, respectively. Our first s-triazine bridged calixarene ligand, which we code as ID2, was obtained from the reaction of the ID1 coded compound with 4-aminobenzoic acid at a 1:2 mole ratio, twice. The ID4 and ID5 coded ligands were obtained from the reaction of the ID3 coded intermediate compound with 4-aminobenzoic acid and 4-hydroxybenzoic acid at a 1:2 mole ratio, respectively. The ID7 and ID8 coded ligands were obtained from the reaction of the ID6 coded intermediate compound with 4-aminobenzoic acid and 4-hydroxybenzoic acid at a 1:2 mole ratio, respectively. [MSalen/Saloph] capped s-triazine bridged calixaren complexes were obtained from the reaction of the ID2, ID4, ID5, ID7 and ID8 codded ligand and the [(MSalen/Saloph)2O] (M=Cr3+, Fe3+ and Co3+) starting complexes in 1,4-dioxane media. The ligands obtained were characterized by using 1H-NMR, FT-IR spectroscopy and elemental analysis techniques. The complexes obtained were characterized by using FT-IR, UV-Vis spectroscopies, elemental analysis, magnetic susceptibility, and TGA-DTA techniques. Metal contents of the complexes were determined by using ICP-AES spectroscopy."
In this study, 2,4-bis((4,6-dichloro-1,3,5-triazin-2-yl)oxy)benzaldehyde, (3,5-bis((4,6-dichloro-1,3,5-triazin-2-yl)oxy)phenyl)methanol and methyl-3,5-bis((4,6-dichloro-1,3,5-triazin-2-yl)oxy)benzoate compounds were obtained by reacting, separately, cyanuric chloride with 2,4-dihydroxybenzaldehyde, 3,5-dihydroxybenzyl alcohol and methyl-3,5-dihydroxybenzoate at 0 °C. Then, s-triazine bridged calixarens codded as ID1, ID3 and ID6 were obtained by reacting the compounds with 2,4-dihydroxybenzaldehide, 3,5-dihydroxybenzylalcohol and methyl-3,5-dihydroxybenzoate, respectively. Our first s-triazine bridged calixarene ligand, which we code as ID2, was obtained from the reaction of the ID1 coded compound with 4-aminobenzoic acid at a 1:2 mole ratio, twice. The ID4 and ID5 coded ligands were obtained from the reaction of the ID3 coded intermediate compound with 4-aminobenzoic acid and 4-hydroxybenzoic acid at a 1:2 mole ratio, respectively. The ID7 and ID8 coded ligands were obtained from the reaction of the ID6 coded intermediate compound with 4-aminobenzoic acid and 4-hydroxybenzoic acid at a 1:2 mole ratio, respectively. [MSalen/Saloph] capped s-triazine bridged calixaren complexes were obtained from the reaction of the ID2, ID4, ID5, ID7 and ID8 codded ligand and the [(MSalen/Saloph)2O] (M=Cr3+, Fe3+ and Co3+) starting complexes in 1,4-dioxane media. The ligands obtained were characterized by using 1H-NMR, FT-IR spectroscopy and elemental analysis techniques. The complexes obtained were characterized by using FT-IR, UV-Vis spectroscopies, elemental analysis, magnetic susceptibility, and TGA-DTA techniques. Metal contents of the complexes were determined by using ICP-AES spectroscopy."
Açıklama
Anahtar Kelimeler
s-Triazine bridged calixarene, s-Triazine bridged calixarene complexes, Schiff Base, Salen, Saloph, s-Triazin köprülü kaliksaren, s-Triazin köprülü kaliksaren kompleksleri, Schiff Bazı, Salen, Saloph