Comprehensive chemical experiment: temperature controlled synthesis, characterization and conversion of mononuclear and binuclear copper complexes
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摘要:化学类专业本科生在理论课学习中，对反应的热力学产物和动力学产物有了一定的理论认识，但目前鲜有实验能够使其直观体会2种产物在制备时的差异．本实验以氯化铜和邻氨基苯甲酰胺为原料，水和乙醇为溶剂，通过仅改变反应温度，分别在60 ℃水浴加热和冰水浴冷却条件下得到了红色的热力学产物二( μ-氯)·二[氯·(邻氨基苯甲酰胺)合铜(Ⅱ)] ( 1)和黄绿色的动力学产物二氯·二(邻氨基苯甲酰胺)合铜(Ⅱ) ( 2)，产率分别为80.4%和76.4%．采用络合滴定法和仪器分析方法对产物进行了表征测试，结果表明在不同温度下可制备2种不同组成、结构和性质的热力学和动力学产物，且在加热条件下，配合物 2可以转化为配合物 1．本设计为化学类相关专业本科生综合实验教学提供了一个成功案例，可加深学生对结构与性能的科学关联以及构效关系的认识和理解．Abstract:Undergraduates in chemistry have a certain theoretical understanding of thermodynamic and kinetic products, but few experiments can demonstrate directly differences in the preparation of these two products．Copper chloride and o-aminobenzamide were used in the present experiment as raw materials, water and ethanol were used as solvents．The reaction temperature only was changed: the thermodynamic red product ( 1) was obtained at 60 ℃ with water bath heating, but the kinetic olive product ( 2) was obtained with ice water bath cooling, with yield of 80.4% and 76.4% respectively．The thermodynamic and kinetic products with different compositions, structures and properties were obtained at different temperatures．In addition, complex 2can be converted to complex 1with heating．This will be an excellent comprehensive-experiment for undergraduates in chemistry．Such experiments will facilitate their understanding of structure-activity relationship．
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表 1组成测定结果
Table 1.Results of composition determination
% 配合物 w(C) w(H) w(N) w(Cu) 配合物1 理论值 31.07 2.98 10.35 23.48 测定值 31.34 3.01 10.26 23.38 配合物2 理论值 41.34 3.96 13.77 15.62 测定值 41.52 4.16 13.71 15.29 
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表 2配合物1的晶体学数据
实验式 C14H16Cl4Cu2N4O2 相对分子质量 541.18 晶系 单斜 空间群 P21/C a/nm 0.82120(1) b/nm 1.38845(2) c/nm 0.81923(1) β/（°） 98.8493(15) V/nm3 0.92296(3) Z 4 GOOF 1.065 R1, w(R2) [I>2σ(I)] 0.0384/0.1034 R1, w(R2) [all data] 0.0397/0.1049 下载:
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