摘要: 在非水溶剂中,β-丙氨酸与苯甲酰基吡唑啉酮反应制备出新氨基酸席夫碱试剂: 1-苯基-3-甲基-4-苯甲酰基吡唑啉酮-5缩β-丙氨酸(HL)。通过回流席夫碱与稀土硝酸盐合成了10种稀土配合物。元素分析与摩尔电导值表明新配合物的组成为[REL2NO3](nH2O(RE=La, Sm , Eu, Tb, Y, n=2; RE=Pr, Nd n=1; RE=Dy, Er, Yb, n=3)。运用红外光谱、紫外光谱、核磁共振谱和荧光光谱对配合物进行了表征。结果表明席夫碱配体以3齿形式配位, RE3+的配位数为8。在可见光区522 nm; 573,584 nm处分别发现Er和Nd配合物的超灵敏跃迁吸收峰。配合物的荧光光谱主要体现稀土离子的f-f跃迁发光,配体的发光影响较小。配合物的荧光强度:ITb>ISm>IEu>IDy。
关键词:稀土;酰基吡唑啉酮缩β-丙氨酸;席夫碱;配合物;光谱
Abstract:In non-aqueous solvent, a new amino-acid schiff base, 1-phenyl-3-methyl-4-benzoyl pyrazolone-5-β-alanine (HL) was synthesized by a reaction of β-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 (4I15/2→2H11/2, 4S3/2) and that of the Nd complex at 573, 584 nm (4I9/2→2G7/2+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.
李锦州,俞志刚,安郁美,杨 昱. 酰基吡唑啉酮缩β-丙氨酸稀土配合物的合成与光谱表征[J]. 光谱学与光谱分析, 2005, 25(09): 1482-1485.
LI Jin-zhou, YU Zhi-gang, AN Yu-mei, YANG Yu. Synthesis and Spectral Characterization of Rare Earth Complexes of Acylpyrazolone-β-Alanine. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2005, 25(09): 1482-1485.
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