DİSPİRO VE TRİSPİRO HALKALI FOSFAZEN TÜREVLERİNİN SENTEZİ, KRİSTAL YAPILARI VE SPEKTROSKOPİK ÖZELLİKLERİNİN İNCELENMESİ
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Tarih
2023-07
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info:eu-repo/semantics/openAccess
Özet
Tez kapsamında, farklı iki dişli sübstitüentler ile 5’ orijinal 8 bileşik sentezlendi. Monospiroferrosenilfosfazen bileşik 1 (monospiroNN) ve 2’nin (monospiroNO), difonksiyonel sübstitüent olan 2,2'-bifenol ile 1:1 stokiometrik oranda reaksiyonlarından, dispiro bileşik 1a ve 2a elde edildi. Monospiroferrosenilfosfazen ve 2,2'-bifenol bileşiklerinin, 1:2 stokiometrik oranda reaksiyonundan trispiro bileşikler 1b ve 2b elde edildi. Dispiroferrosenilfosfazen 3 (dispiroNO.NO) bileşiğinin 2,2'-bifenol ile 1:1 stokiometrik oranda reaksiyonundan ise trispiro bileşik 3a sentezlendi. Ayrıca cis- ve trans-dispiroferrosenilfosfazen [dispiroNN.NN; dispiro(N-methyl-1,3-propandiamino) [N-(1-ferrosenilmetil)]-6,6-diklorosiklotrifosfazatrien] bileşikleri de çıkış maddesi olarak sentezlendi ve 2,2'-bifenol ile 1:1 stokiometrik oranda reaksiyonu ile trispiro ürün elde edilmek istendi. Ancak çözücü değişikliğine ve reaksiyon süresinin uzatılmasına rağmen beklenen trispiro ürünlerin oluşmadığı gözlendi. Sentezlenen bileşiklerin tamamı, kolon kromatografisi yöntemi ile farklı yürütücü fazlar kullanılarak saflaştırıldı. Elde edilen orjinal bileşiklerin yapıları (1a, 1b, 2a, 2b ve 3a) elementel analiz, FTIR, 1H-, 13C-, 31P-NMR tekniklerinden yararlanılarak karakterize edildi. Uygun tek kristali elde edilen bileşik 1a ve 2b nin katı hal yapıları, X-ışınları kristallografi tekniği ile aydınlatıldı.
In this thesis, 8 compounds with different bidentate substituents were synthesized, 5 of which were original. The reactions of monospiroferrocenylphosphazene compounds 1 (monospiroNN) and 2 (monospiroNO) with the difunctional substituent 2,2'-biphenol in a 1:1 stoichiometric ratio yielded dispiro compounds 1a and 2a. From the reaction of monospiroferrocenylphosphazene and 2,2'-biphenol in 1:2 stoichiometric ratio, trispiro compounds 1b and 2b were obtained. Trispiro compound 3a was synthesized from the reaction of dispiroferrocenylphosphazene 3 (dispiroNO.NO) with 2,2'-biphenol in 1:1 stoichiometric ratio. In addition, cis- and trans-dispiroferrocenylphosphazene [dispiroNN.NN; dispiro (N-methyl-1,3-propanediamino) [N- (1-ferrocenylmethyl)] -6,6-dichlorocyclotriphosphazatriene] compounds were synthesized as starting material and the reaction with 2,2'-biphenol in a stoichiometric ratio of 1:1 was carried out to obtain trispiro products. However, despite the change of solvent and extension of the reaction time, the expected trispiro products were not formed. (The 31P-NMR spectrum data were evaluated). All of the synthesized compounds were purified by column chromatography using different mobile phases. The structures of the original compounds obtained (1a, 1b, 2a, 2b and 3a) were characterized by elemental analysis, FTIR, 1H-, 13C-, 31P-NMR techniques. Suitable single crystals of compounds 1a and 2b solid state structures were elucidated by X-ray crystallography technique."
In this thesis, 8 compounds with different bidentate substituents were synthesized, 5 of which were original. The reactions of monospiroferrocenylphosphazene compounds 1 (monospiroNN) and 2 (monospiroNO) with the difunctional substituent 2,2'-biphenol in a 1:1 stoichiometric ratio yielded dispiro compounds 1a and 2a. From the reaction of monospiroferrocenylphosphazene and 2,2'-biphenol in 1:2 stoichiometric ratio, trispiro compounds 1b and 2b were obtained. Trispiro compound 3a was synthesized from the reaction of dispiroferrocenylphosphazene 3 (dispiroNO.NO) with 2,2'-biphenol in 1:1 stoichiometric ratio. In addition, cis- and trans-dispiroferrocenylphosphazene [dispiroNN.NN; dispiro (N-methyl-1,3-propanediamino) [N- (1-ferrocenylmethyl)] -6,6-dichlorocyclotriphosphazatriene] compounds were synthesized as starting material and the reaction with 2,2'-biphenol in a stoichiometric ratio of 1:1 was carried out to obtain trispiro products. However, despite the change of solvent and extension of the reaction time, the expected trispiro products were not formed. (The 31P-NMR spectrum data were evaluated). All of the synthesized compounds were purified by column chromatography using different mobile phases. The structures of the original compounds obtained (1a, 1b, 2a, 2b and 3a) were characterized by elemental analysis, FTIR, 1H-, 13C-, 31P-NMR techniques. Suitable single crystals of compounds 1a and 2b solid state structures were elucidated by X-ray crystallography technique."
Açıklama
Anahtar Kelimeler
Spirofosfazen, 2, 2'-bifenol, X-ışınları., Spirophosphazene, 2, 2'-biphenol, X-rays
