节点文献
4,4′-联苯-3,3′-二(2,4-戊二酮)的合成与热谱研究
Study on synthesis and thermograms of 3,3′-(biphenyl-4,4′-diyl)dipentane-2,4-dione
【摘要】 以4,4′-二(氯甲基)联苯和2,3-丁二酮-亚磷酸三甲酯(1∶1)加合物为原料合成了标题化合物,采用核磁共振谱、质谱、红外光谱和紫外可见光谱对化合物进行结构表征。在静态空气气氛中用热重-差示扫描量热分析法(TG-DSC)对其进行了热分析研究:168~436℃之间质量损失76.67%,最后的固体残留物为联苯骨架不完全燃烧的残留物。在272℃有一个放热峰,在210、302℃分别出现强吸热峰。结果表明该固态化合物在168℃以下很稳定。
【Abstract】 In this paper,3,3′-(biphenyl-4,4′-diyl)dipentane-2,4-dione was synthesized using 4,4′-bis(chloromethyl)biphenyl and 2,2,2-trimethoxy-4,5-dimethyl-1,3,2-dioxaphospholene as starting materials.Its molecule structure was characterized by 1HNMR,MS,IR and UV-Vis spectra.The thermal properties of 3,3′-(biphenyl-4,4′-diyl)dipentane-2,4-dione were studied based on the TG-DTG and DSC-DDSC analyses in a static air atmosphere.In a temperature range from 168 ℃ to 436 ℃,a mass loss of 76.67% was observed.The last solid residue was considered generally as the remnants of biphenyl skeleton after incomplete combustion.The maximum peak of heat release at 272 ℃ in DTG was resulted from exothermal decomposition reactions.The maximum peak of heat absorption at 210 ℃ and 302 ℃ in DSC was resulted from endothermic reactions,respectively.The test results showed the compound had higher thermal stability at 168 ℃.
【Key words】 3,3′-(biphenyl-4,4′-diyl)dipentane-2,4-dione; synthesis; characterization; thermal analysis;
- 【文献出处】 化学试剂 ,Chemical Reagents , 编辑部邮箱 ,2009年11期
- 【分类号】O621.13
- 【被引频次】4
- 【下载频次】207