苯甲醇合成苯甲酸乙酯综合制备实验的课程思政设计
刘玲, 王海滨, 强根荣
【大学化学】doi: 10.3866/PKU.DXHX202304080
将苯甲酸合成与苯甲酸乙酯制备两个经典实验改造为综合实验,并以改进合成过程实现绿色、高效转化为案例,引导学生通过查阅文献,综合分析合成过程,指出原合成方法存在的问题和不足,提出改进的建议,在此过程中,引导学生将法律法规、实验规范、学科伦理、绿色理念、环保和可持续发展理念等融入实验的设计和实施全过程,使学生在受到基本操作训练的同时得到素质的全面提升。
关键词: 苯甲醇, 苯甲酸, 苯甲酸乙酯, 有机化学实验, 绿色化学, 课程思政
4-羟基苯乙酮制备对乙酰氨基酚的两步合成实验设计
匡永清, 刘劼, 冯见君, 杨文, 蔡双莲, 史玲
【大学化学】doi: 10.12461/PKU.DXHX202403012
设计了由4-羟基苯乙酮制备对乙酰氨基酚的两步合成实验,并应用于本科教学。先由4-羟基苯乙酮与羟胺缩合产生4-羟基苯乙酮肟,再由三聚氯氰催化4-羟基苯乙酮的Beckmann重排反应得到对乙酰氨基酚。实验应用了回流、萃取、干燥、过滤、旋转蒸发、薄层色谱和柱层析等重要有机实验操作,可综合训练学生的有机合成技术。通过制备具有重要医学和经济价值的目标化合物,向学生展示了有机合成技术在实际生活中的应用,有利于提高他们学习有机化学的兴趣。Beckmann重排采用了有机小分子催化剂,有助于学生加深理解有机催化的意义和Beckmann重排反应的机理。
关键词: 对乙酰氨基酚, 酮肟化, Beckmann重排, 有机催化
一例多齿席夫碱构筑的Tb2配合物的结构、荧光性质及生物活性
马鑫, 孙娅, 孙楠, 康倩, 张佳佳, 朱瑞涛, 高晓丽
【无机化学学报】doi: 10.11862/CJIC.20230357
使用多齿希夫碱配体H4L(H4L=N',N″-((1E,1'E)-(1,10-菲咯啉-2,9-二酰基)双(亚甲基)双(2-羟基苯甲酰肼))与Tb(acac)3·2H2O反应(acac-=乙酰丙酮根),通过溶剂热法,设计并合成了一例结构新颖的双核铽配合物[Tb2(L)(H2L)]·2CH3OH·CH3CN (1),并研究了该配合物的结构、荧光性质及生物活性。单晶X射线衍射分析表明该配合物主要含有2个Tb离子和2个失去不同质子的配体离子(L4-和H2L2-)。中心Tb1和Tb2离子都是九配位的,其几何构型呈现扭曲的呼啦圈形。固体荧光实验测试结果表明:该配合物在室温下表现出Tb离子的荧光特征发射峰。生物活性研究表明,与配体H4L和稀土离子相比较,配合物具有更强的抗菌活性。采用紫外可见光谱法、循环伏安法、凝胶电泳法和荧光光谱法研究了该配合物与小牛胸腺DNA之间的相互作用,结果表明配合物主要以插入作用的方式与小牛胸腺DNA结合。
关键词: Tb2配合物, 生物活性, DNA作用, 荧光性质, 晶体结构
Two Ni-based frameworks with helices and dinuclear units constructed from semi-rigid carboxylic acid and imidazole derivatives
Xiaoru LIU, Jinlian SHI, Yajia ZHENG, Shuangcun MO, Zhongxuan XU
【无机化学学报】doi: 10.11862/CJIC.20240328
Under hydrothermal conditions, semi-rigid 4-(1-carboxyethoxy)benzoic acid (H2cba) and Ni(Ⅱ) ions reacted with imidazole derivatives 1,4-di(1H-imidazol-1-yl)benzene (1,4-dib) and 4,4'-di(1H-imidazol-1-yl)-1,1'-biphenyl (4, 4' dib) to form complexes {[Ni(cba)(1, 4 dib)(H2O)0.5] ·0.5H2O}n (HU21) and {[Ni(cba)(4, 4' dib)(H2O)0.5] · 0.5H 2O}n (HU22), respectively. Singlecrystal X-ray diffraction analysis revealed that both complexes HU21 and HU22 contain binuclear [Ni2(CO2)2(H2O)]2+ units, which are further bridged together via cba2- anions to form 1D [Ni2(H2O)(cba)2]n chains in HU21 and HU22. In addition to the [Ni2(H2O)(cba)2]n chains, large right-handed and lefthanded helical chains were constructed by Ni(Ⅱ) ions, water molecules, and 1,4-dib ligands in HU21, with diameters of up to 1.6 nm along the b-axis. These helical chains are further joined together in a 1∶1 ratio to form a 3D framework. Subsequently, the [Ni2(H2O)(cba)2]n chains are incorporated into the 3D framework to build a six-connected dense network with a point symbol of (44.611) in HU21. In complex HU22, left-and right-handed helical chains were also observed. However, unlike the 3D framework constructed by helical chains in HU21, these helical chains in HU22 can only form a 2D layer. Adjacent layers are packed together in an ABAB pattern to form a six-connected framework in the presence of [Ni2(H2O) (cba)2]n chains. UV-Vis absorption experiments indicated that complexes HU21 and HU22 are semiconductor materials with strong light absorption capacities in the ultraviolet and visible regions. Moreover, magnetic experiments showed that HU21 and HU22 exhibit similar antiferromagnetic behaviors.
关键词: Ni-based complex, binuclear unit, helical chain, semiconductor material, antiferromagnetic property

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