4-酰代-双(1,3-二苯基-5-吡唑酮)螯合剂的合成与表征

于 90℃ ,以二氧六环为溶剂 ,Ca(OH) 2 为缩合剂 ,由 1,3 二苯基 5 吡唑酮分别与戊、己和癸二酰氯作用 (量比为 2∶1) ,合成了三种新的 β 二酮螯合剂 4 酰代 双 (1,3 二苯基 5 吡唑酮 )(各以符号P、H和D表示 ) ,收率为 6 5 .5 %、6 7.4%和 6 1.0 %。通过元素分析、红外光谱和核磁共振氢谱证实了产物的结构。测定了以它们为配体的Tb(Ⅲ )配合物的荧光光谱 ,结果表明 :这三种化合物的Tb(Ⅲ )配合物的荧光强度高于 4 酰代 双 (1 苯基 3 甲基 5 吡唑酮 )的Tb(Ⅲ )配合物 ;这三种化合物的Tb(Ⅲ )配合物荧光强度的顺序为P >H >D。

Synthesis and Characterization of 4-Acyl-bis(1,3-diphenyl-5- pyrazolone) Chelating Agents

Three new β-diketone chelating agents(showed as P,H and D),4-acyl-bis(1,3-diphenyl-5-pyrazolones),were synthesized by treating a solution of 1,3-diphenyl-5-pyrazolone in dioxane containing suspended calcium hydroxide as condensing agent at 90 ℃ with pentanedioyl,hexanedioyl and decanedioyl dichloride,the yields being 65.5%，67.4% and 61.0% respectively.Structures of the products were confirmed by elementary analysis,FT-IR and 1 HNMR spectra.The fluorescence spectra of Tb(Ⅲ) complexes prepared with the three compounds as ligands were determined.It was indicated that the fluorescence intensities of the above complexes were higher than that of Tb(Ⅲ) complexes with 4-acyl-bis(1-diphenyl-3-methyl-5-pyrazolones) and that the descending order of fluorescence intensities of the above complexes was P>H>D.