1-苯基-5-苯基吡唑基-3-氧乙酸乙酯的合成及晶体结构

Synthesis and Structure Characterization of Ethyl 1-Phenyl-5-Phenylpyrazol-3-Oxyacetate

以肉桂酸甲酯与苯肼为原料,合成得到了1-苯基-5-苯基-3-吡唑烷酮,再经氧化得到1-苯基-5-苯基-3-羟基吡唑,最后与溴乙酸乙酯反应,得到1-苯基-5-苯基吡唑基-3-氧乙酸乙酯,利用溶剂挥发法得到标题化合物的单晶。用元素分析、~1H-核磁共振谱进行了表征,用X-射线单晶衍射分析仪测定了其晶体结构,结果表明：标题化合物晶体属于正交晶系,所属空间群为Pbca,a=1.114 3（2）nm,b=1.573 3（3）nm,c=1.948 4（4）nm,α=90.00°,β=90.00°,γ=90.00（,Dc=1.158g/cm3,Z=8,F（000）=1 360,最终偏差因子分别为R=0.138 3,wR=0.1665。

Ethyl 1-phenyl-5-phenylpyrazol-3-oxyacetate was prepared by reaction of ethyl bromoacetate and 1-phenyl-5-phenyl-3-hydroxypyrazol which was synthesized through the reaction of methyl cinnamate and phenyl hydrazine. The crystal of ethyl 1-phenyl-5-phenylpyrazol-3-oxyacetate was been obtained by slowly evaporation of solution. Meanwhile, analyses are made of elements, nuclear magnetism characterization and X-ray single crystal diffraction. The outcome of crystal structure analysis shows that the crystal is orthorhombic system, Pbca space group, a=1. 114 3（2）nm, b=1. 573 3（3）nm, c=1. 948 4（4）nm,α=90. 00＆#176;,β=90. 00＆#176;,γ=90. 00（, Dc=1. 158 g/cm3 , Z=8, F（000） =1 360. The final deviation factors are R=0. 1383, wR=0. 1665 separately.