综合创新型实验:乙胺嘧啶合成的设计与教学实践

乙胺嘧啶(商品名:达拉匹林)是一种抗寄生虫药物,改进了合成方法,并设计转化为创新型综合教学实验。从对氯苯乙腈出发,使用丙酸乙酯为酰化试剂,在叔丁醇钾作用下得到烯醇前体。在三甲基氧鎓四氟硼酸盐(Me3O·BF4,Meerwein盐)和碱作用下进行选择性甲基化反应得到烯醇甲醚后,与胍在碱性条件下环化得到最终产物达拉匹林,并通过红外光谱、核磁共振对其结构进行表征。改进后的实验方法具有重现性好、毒性低、操作方便、实验微型化等优点。实验过程中不仅提升了学生的实验技能和科研思维,更提高了学生的创新能力和绿色环保意识。     

微视频技术在基础化学实验教学中的实践应用

以高校基础化学实验"从海带中提取碘""三草酸合铁（Ⅲ）酸钾的制备"为例，分别探讨了微视频技术在化学基本操作实验和综合设计型实验中的具体应用；此外，举例说明利用Flash软件制作的虚拟微视频可以在仪器分析实验中清晰地再现仪器真实操作中的每一个步骤，弥补了学生在实验前无法实际操作仪器的不足。实践证明，微视频技术的应用，丰富了基础化学实验教学模式，增强了学生自主学习的能力和动手能力，提高了实验成功率和实验教学效果。     

综合设计性专业实验:离子液体[BMIM]Br的制备及在柴油脱硫中的应用

在微波辅助下合成、纯化了离子液体溴化1-甲基-3-丁基咪唑[BMIM]Br，测定了产率和纯度，并使用FTIR和1HNMR进行了产物结构表征；以[BMIM]Br为萃取剂对催化裂化和加氢裂化柴油进行超声辅助萃取脱硫，并测定了脱硫率；在反应条件优化、测试方法优化、脱硫选择性等方面设置了多个开放性设计实验。该实验项目融合精细化工和石油化工方向，在促进学生知识体系跨界，全面训练综合实验技能，培养学生解决实际问题能力以及科研能力形成等方面作用明显；实验项目以模块化设置，符合"绿色实验"原则。     

4,4'-[(2,2-二苯乙烯)-1,1-双(4,1-亚苯基)]二吡啶的合成、表征及其聚集诱导发光性能研究

以提升学生的实验操作及创新能力为目的的综合化学实验，采用简单的2步法（缩合和Suzuki反应）合成了一种具有聚集诱导发光性能的化合物4，4'-[（2，2-二苯乙烯）-1，1-双（4，1-亚苯基）]二吡啶（简称2Py-TPE）。利用过滤、洗涤、萃取、干燥和柱层析等常用的有机分离操作手段对该化合物进行纯化；使用核磁共振仪、高分辨质谱仪、红外光谱仪及稳态瞬态荧光光谱仪对其进行结构表征和聚集诱导发光性能研究。该实验不仅可以促使学生了解以四苯乙烯衍生物为代表的聚集诱导发光材料的研究现状，而且能够培养学生的综合实验能力和科学探究能力。     

Advanced statistical evaluation of the complex formation constants from electrophoretic data II: Diastereomeric ion-pairs of (R,S)-N-(3,5-dinitrobenzoyl)leucine and tert-butylcarbamoylquinine

Intermolecular association and ion-pair formation, respectively, between a cationic chiral selector, viz. o-9-(tert-butylcarbamoyl) quinine (CQN), and the both enantiomers of anionic N-(3,5-dinitrobenzoyl)leucine, (R)-DNB-Leu and (S)-DNB-Leu, were investigated by affinity capillary electrophoresis (ACE). Thus, binding constants of the both diastereomeric ion-pairs, (R) and (S)-DNB-Leu/CQN associates, were determined by different experimental setups and correction of nonlinear effects. A reciprocal setup was employed for the high-affinity (S)-enantiomer, and the experimental mobility data obtained for CQN at variable (S)-DNB-Leu concentrations in the background electrolyte were linearized and evaluated by advanced statistical model. A binding constant of K_S=125.1 l mol⁻¹ was afforded. The constant for the (R)-enantiomer, which is outside the range suitable for direct affinity CE, was obtained from indirect affinity CE utilizing the separation of the DNB-Leu racemate at a single appropriate CQN concentration in the BGE (resolution method) taking advantage of the known constant for the (S)-enantiomer yielding a binding constant of K_R=2.51 l mol⁻¹. Thereby, the so-called “constant time method” was adopted for the required precise measurement of the effective mobilities of the both enantiomers. A combined approach of reciprocal affinity CE with racemic DNB-Leu as additive and the resolution method confirmed the results. The resulting constants evidence excellent enantioselectivity of the tert-butylcarbamoyl derivative of the cinchona alkaloid quinine as chiral selector for N-(3,5-dinitrobenzoyl) derivatives of amino acids.     

“线上线下-虚实结合”在有机化学实验教学中的应用探索——以正溴丁烷的制备实验为例

In response to the impact of the Covid-19 epidemic on organic chemistry laboratory teaching, this article analyzes and discusses the current limitation of traditional organic chemistry laboratory teaching. Taking the "preparation of n-bromobutane" as an example, a new "online-offline and virtual-actual combination" teaching mode with the combination of "Tencent Meeting, MLabs, laboratory and WeChat group" is introduced. The practice of the new mode of teaching includes the following steps: pre-class online guiding by teacher, student preview and practice based on the virtual simulation platform, students and teacher discussion and operation in laboratory, and post-classcomprehensive assessment and Q&A", and good teaching effects have been received. It is significant in cultivating and improving the independent innovation and practical ability, and provides reference for the organic chemistry laboratory teaching reform and also lays a foundation for the construction of "outstanding course" of organic chemistry.     

青藏高原油菜蜂花粉中黄酮类物质的提取与开发的实验设计

本文根据作者从事的青藏高原油菜蜂花粉中黄酮类物质的提取和开发应用的研究，探讨了综合实验的设计，把科学研究引入到实验教学中，将会极大地促进高校的实验教学改革．     

亚铁法处理大型高炉煤气洗涤水中氰化物的实验研究

采用亚铁法处理高炉煤气洗涤水，并用正交实验设计方法设计实验。根据正交实验结果分析和单因素实验得出：硫酸亚铁可以有效除去高炉煤气洗涤水中的氰化物；最佳反应条件为：T=30℃，pH=6，α=3．5，t，=40min，td=35min；影响因素顺序为：r〉α〉pH〉td〉tr。     

莠去津在填充土柱中的运移

用土柱实验模拟莠去津在土壤中的运移、实验结果表明相当浓度的莠去津被淋溶到土柱的底部，说明莠去津对地下水存在很大威胁、应用CXTFIT的平衡与非平衡模型模拟莠去津在土柱中的运移，模拟结果表明CXTFIT的非平衡模型能很好地模拟莠去津的穿透曲线．由CXTFIT率定得到的莠去津在土柱实验中的吸附和降解参数和从批次实验得到的吸附和降解参数有较好的一致性．     

电氧化法处理高浓度酚钠废水

为了改善强碱性废水的可生化性,采用电氧化法处理高浓度酚钠废水.结果表明：电氧化法对废水的色度和S（重铬酸钾化学耗氧量）具有良好的去除效果,电解过程中余氯的产生对色度和S的去除有决定性作用.实验确定的高浓度酚钠废水电氧化处理条件是：电流密度为714 A/m^2、电压为10 V、电解时间为30min,采用中和→电氧化→生化工艺去除色度和S.