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酰基吡唑啉酮-β-丙氨酸稀土配合物的合成与光谱表征

[Synthesis and spectral characterization of rare earth complexes of acylpyrazolone-beta-alanine].

作者信息

Li Jin-zhou, Yu Zhi-gang, An Yu-mei, Yang Yu

机构信息

Department of Chemistry, Harbin Normal University, Harbin 150080, China.

出版信息

Guang Pu Xue Yu Guang Pu Fen Xi. 2005 Sep;25(9):1482-5.

PMID:16379296
Abstract

In non-aqueous solvent, a new amino-acid schiff base, 1-phenyl-3-methyl-4-benzoyl pyrazolone-5-beta-alanine (HL) was synthesized by a reaction of beta-alanine with benzoylpyrazolone, and its ten rare earth complexes were obtained from refluxing a solution of schiff base and rare earth nitrates. On the basis of elemental analysis and molar conductance, the general formula of the complexes, [REL2NO3] nH2O (RE=La, Sm, Eu, Tb, Y, n=2; RE=Pr, Nd, n = 1; RE=Dy, Er, Yb, n=3), is given. These were characterized by IR, UV-Visible, 1H NMR, 13C NMR and fluorescence. The results show that the schiff base is a tridentate ligand, and the rare earth ions exhibit a coordination of eight in the complexes. In visible spectra, the supersensitive transitions of the Er complex at 522 nm (4 I15/2 -->2 H11/2, 4 S3/2 ) and that of the Nd complex at 573, 584 nm (4I9/2 -->2 G7/2 + 4G5/2) can be observed. Fluorescence of the complexes was produced principally by f-f transition of central ion RE3+, and the ligand has little influence on lightening role. The order of relative intensity of fluorescence of the complexes is ITb > ISm > IEu > IDy.

摘要

在非水溶剂中,通过β-丙氨酸与苯甲酰吡唑酮反应合成了一种新型氨基酸席夫碱1-苯基-3-甲基-4-苯甲酰基吡唑啉酮-5-β-丙氨酸(HL),并通过席夫碱与稀土硝酸盐溶液回流得到了其十种稀土配合物。基于元素分析和摩尔电导率,给出了配合物的通式[REL2NO3] nH2O(RE = La、Sm、Eu、Tb、Y,n = 2;RE = Pr、Nd,n = 1;RE = Dy、Er、Yb,n = 3)。通过红外光谱、紫外可见光谱、1H核磁共振、13C核磁共振和荧光对这些配合物进行了表征。结果表明,席夫碱是一种三齿配体,稀土离子在配合物中呈现八配位。在可见光谱中,可以观察到铒配合物在522 nm(4I15/2→2H11/2,4S3/2)处以及钕配合物在573、584 nm(4I9/2→2G7/2 + 4G5/2)处的超灵敏跃迁。配合物的荧光主要由中心离子RE3+的f-f跃迁产生,配体对发光作用影响较小。配合物荧光相对强度的顺序为ITb > ISm > IEu > IDy。

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