【摘要】 以无水Na2CO3为催化剂、苯为溶剂,对氯苯甲醛与乙二胺经回流分水反应得到对氯苯甲醛-乙二胺席夫碱(1)。再将1与Cu(ClO4)2.6H2O在乙醇溶剂中回流反应,反应液冷至室温析出紫色固体化合物2。2溶于丙酮中,室温放置缓慢蒸发溶剂析出标题化合物3。经元素分析、红外光谱(IR)和X-衍射单晶衍射测定,确定了3的立体化学结构。3的晶体属单斜晶系,P2(1)空间群,分子式为C16H38Cl2CuN4O11,Mr=596.94。晶胞参数:a=8.1429(11),b=15.504(2),c=10.6180(14),β=93.522(2)°,V=1337.9(3)3,Z=2,Dc=1.482 Mg/m3。最终偏差因子R1=0.0566,wR2=0.1446[I>2σ(I)]。更多还原

【Abstract】 In benzene solvent,4-chlorobenzaldehyde-ethylenediamine Schiff base(1) was synthesized by the reaction of 4-chlorobenzaldehyde and ethylenediamine catalyzed by anhydrous Na2CO3 under refluxing in a Dean-Stark apparatus for water separation.Subsequently compound 1 reacted with Cu(ClO4)2·6H2O in ethanol solvent under refluxing,to form a purple solid 2 after cooling to room temperature.compound 2 was dissolved in acetone the solvent was slowly evaporated under room temperature and then the title compound 3 was obtained.The stereochemistry structure of compound 3 was determined by elemental analysis,IR spectra and single-crystal X-ray diffraction.The crystal of compound 3 was attributed to monoclinic system and P2(1) space group.Molecular formula:C16H38Cl2CuN4O11,Mr=596.94.The crystal lattice parameters are a=8.1429(11) ,b=15.504(2) ,c=10.6180(14) ,β=93.522(2)°,V=1337.9(3) 3,Z=2,Dc=1.482 Mg/m3.The final deflection factors R1=0.0566,wR2=0.1446[I>2σ(I)].更多还原