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对烷氧苯基二茂铁基β-二酮及其配合物的合成与表征

Synthesis and Characterization of P-Alkoxylphenyl Ferrocenyl β-Diketone and Its Complex

【作者】 商亚东

【导师】 李保国;

【作者基本信息】 内蒙古大学 , 有机化学, 2007, 硕士

【摘要】 随着科学技术的飞速发展,液晶在科技和工业上的应用更加广泛和深入。极化的二茂铁衍生物也已经成为功能材料研究的一个重要课题,其中β-二酮类二茂铁过渡金属配合物就有良好的金属有机液晶性质,而且具有稳定性好、相转移温度低等特点。本文通过酮酯缩合合成了5种对烷氧苯基二茂铁基β-二酮配体,并分别与部分过渡金属钴、镍、铜、锌形成配合物,这些化合物都经过元素分析、红外光谱和核磁共振氢谱进行了表征。在溶剂石油醚和二氯甲烷中通过重结晶的方法培养出对辛氧基苯基二茂铁基β-二酮及其铜配合物的单晶,单晶结构经过四圆衍射仪测定,β-二酮单晶数据如下:单斜晶系,P21/c空间群,a=18.5985(14)(?),b=10.5710(8)(?),c=12.0814(10)(?),a=90°,β=95.1050(10)°,γ=90°,V=2365.8(3)(?)3,Z=4,Dc=1.293mg·m-3,μ=0.662mm-1,F(000)=976。铜配合物单晶数据如下:单斜晶系,P21/c空间群,a=18.5985(14)(?),b=10.5710(8)(?),c=12.0814(10)(?),α=90°,β=95.1050(10)°,γ=90°,V=2365.8(3)(?)3,Z=4,Dc=1.293 mg·m-3,μ=0.662 mm-1,F(000)=976。通过示差扫描量热法(DSC)和偏光显微镜法(POM)测试化合物的液晶行为,最终确定分子长径比大于4的十八碳烷氧基苯基二茂铁基β-二酮的铜和锌的配合物属于近晶型热致液晶。

【Abstract】 With the development of the scientific technology, liquid crystal has been usedwidely in science and industry. In particular, ferrocene-containingβ-diketonetransition metal complexes showed remarkable thermal stability and mesomorphiccharacter.The ketone-ester condensation of actylferrocene and methyl p-alkoxy benzonateafforded the five novel p-n-alkoxylphenyl ferrocenylβ-diketone compound andthese Iigands afforded some complexes with transition metal (Co,Ni,Cu,Zn), allcompounds has been characterized by element analysis, IR and 1H NMRspectroscopies.Two kinds of crystals was recrystallized using petroleum ether anddichloromethane by slow evaporation at room temperature. The crystal structure oftheβ-diketone and its complex has also been determined by single crystal X-raydiffraction technique. It was found that theβ-diketone compound crystallized in amondinic P21/c space group and a=18.5985(14) (?), b=10.5710(8) (?), c=12.0814(10) (?), a=90°,β= 95.1050(10)°,γ= 90°, V= 2365.8(3) (?)3, Z=4, Dc=1.293 mg·m-3,μ=0.662 mm-1, F(000)=976. It was found that the complexcrystallized in a mondinic P21/c space group and a=21.437(2) (?), b=9.7129(10)(?), c=25.935(3) (?), a=90°,β=99.085(2)°,γ=90°, V=5332.5(10)(?)3, Z=4,Dc=1.329 mg·m-3,μ=1.079 mm-1, F(000)=2228. Their phase transitions of liquid crystal were studied by polarizing Opticalmicroscope (POM)and differential scanning calorimetry(DSC). We foundp-octadecanalkoxyl phenyl ferrocenylβ-diketone and its complex of copper(Ⅱ) aresmectic thermotropic liquid crystal because its length-diameter ratio is above four.

  • 【网络出版投稿人】 内蒙古大学
  • 【网络出版年期】2007年 06期
  • 【分类号】O641.4
  • 【被引频次】1
  • 【下载频次】159
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