基于Co(II)配合物前驱体的微纳米Co3O4功能材料的研究进展
朱红林，郑岳青*
(宁波大学应用固体化学研究中心 化学合成与绿色应用研究所，浙江 宁波 315211)
摘要：金属有机骨架(MOFs)是由有机配体和金属节点通过自组装形成的一类具有周期性结构和较大比表面积的材料。目前，选择MOFs材料作为前驱体，经高温焙烧合成纳米金属氧化物或纳米复合金属氧化物材料是一大研究热点。综述了近年来以Co基配位聚合物为前驱体制备纳米Co3O4或Co3O4/碳纳米复合材料的方法，以及Co3O4纳米材料在锂离子电池负极材料、超级电容器、电催化析氧反应、气敏材料及催化剂材料等研究领域的应用，并对其今后的发展进行了展望。
关键词：金属有机骨架化合物；Co基配合物；前驱体；纳米材料；Co3O4
中图分类号：O614.8 文献标识码：A 文章编号：0258-3283（2017）
Progress on Micro/Nano Co3O4 Functional Materials Derived from Co-Coordination Complexes ZHU Hong-lin, ZHENG Yue-qing*(Research Center of Applied Solid State Chemisty, Chemistry Institute for Synthesis and Green Application, Ningbo University, Ningbo 315211, China), Huaxue Shiji, 2017, 39(6)
Abstract：The metal-organic frameworks (MOFs), which possess a periodic network structure with self-assembled by organic ligand and metal node, and ultra-high surface area, have been utilized as precursors via calcination process to generate structured nanoporous metal oxide or porous metal oxide/carbon materials composite. Fabrication of the metal oxides materials from MOFs precursors has attracted intensive research attention in the materials field. In this paper, we summarized the recent progresses of Co3O4 nanomaterials derived from precursive Co-based coordination polymers. We have reviewed the synthesis methods for metal oxide or porous metal oxide/carbon materials composite. In addition, we also summarized the applications of Co3O4 nanomaterials in the field such as lithium ion battery, supercapacitor, oxygen evolution reaction (OER) catalyst, gas sensing materials and catalysts materials. Furthermore, the future development and challenges of Co3O4 materials derived from coordination complexes were discussed.
Key words：metal-organic frameworks (MOFs); Co-coordination complex; precursor; nanomaterials; Co3O4
乳酸-钴( II )-1，10-菲啰啉三元配合物与DNA结合的光谱与电化学研究
邱玮玮，王庆华，林海彬，汪庆祥*
(福建省闽南师范大学 化学与环境学院，福建 漳州 363000)
摘要：以1, 10-菲啰啉（phen）和乳酸为配体合成了三元钴配合物[Co(phen)(la)2]。采用紫外光谱、循环伏安法、计时库仑法和微分脉冲伏安法等考察了其与鲱鱼精天然DNA的相互作用。紫外光谱实验显示，在[Co(phen)(la)2]中加入DNA后，配合物在270 nm处的紫外特征吸收峰出现明显的减色效应，并伴随红移，表明[Co(phen)(la)2]可通过其phen配体插入DNA中相邻碱基对。循环伏安法和计时库仑法进一步表明，与DNA 结合后，复合物在水溶液中扩散系数降低，从而导致电化学信号减弱。微分脉冲伏安实验显示，[Co(phen)(la)2]氧化峰电流与DNA浓度在2.66×10–5 ～ 1.34×10–4 mol/L范围内呈良好线性关系，[Co(phen)(la)2]可作为一种潜在的DNA检测探针。
关键词：钴配合物；DNA；电化学；嵌插作用
中图分类号： 文献标识码：A 文章编号：0258-3283（2017）
Spectroscopic and Electrochemical Investigation on the DNA-binding Property of a Cobalt (II) Complex with Mixed-ligands of Lactic Acid and 1, 10-Phenathroline QIU Wei-wei, WANG Qing-hua, LIN Hai-bin, WANG Qing-xiang*（College of Chemistry and Environment Science, Minnan Normal University, Zhangzhou 363000, China), Huaxue Shiji, 2017, 39(6)
Abstract: A ternary cobalt complex [Co(phen)(la)2] has been synthesized by the reaction of cobalt salt with 1, 10 - phenanthroline (phen) and lactic acid. The interaction of the complex with natural fishsperm DNA was investigated by cyclic voltammetry, UV absorbance spectroscopy, chronocoulometry and differential pulse voltammetry. The results of UV absorbance spectroscopy revealed that DNA could induce the hypochromic effect and red-shift of characteristic absorbance peak of the complex, suggesting that the cobalt complex can interact with DNA via a typical intercalation binding mode. The cyclic voltammetry and chronocoulometry further showed that the diffusion coefficient of the complex was decreased after the interaction of the complex with DNA. Quantitative analysis by differential pulse voltammetry demonstrated that the cobalt complex can be successfully used for the detection of DNA as an electrochemical probe, with a linear response range of 2.66×10–5 ～ 1.34×10–4 mol/L.
Key words: cobalt complex; DNA; electrochemistry; intercalation
硅胶负载硫酸（SSA）催化合成不对称芳基硫醚类化合物
及其抗真菌活性和分子对接研究
钟一凡，韩晓燕，李生彬，齐慧，周增辉，宋亚丽*
（河北大学 药学院 河北省药品质量控制重点实验室，河北 保定 071002）
摘要：通过固载催化剂硅胶硫酸（SSA）催化苯硫酚、芳香醛和5, 5-二甲基-1, 3-环己二酮进行多组分反应得到不对称芳基硫醚类化合物3-羟基-5，5-二甲基-2-[(1-苯硫基-1-苯基)]甲基-环己烯酮，SSA催化使反应产率更高且催化剂可重复使用。通过催化剂量、温度和投料物质的量比优化得到了最佳反应条件。目标化合物通过IR、1HNMR、13CNMR和HR-MS对结构进行确证，初步生物活性测试表明部分化合物具有抗新生隐球菌和白色念珠菌的活性。同时对3-羟基-5，5-二甲基-2-[1-(2-氟苯硫基-1-苯基) ]甲基-2-环己烯酮和白色念珠菌的N-肉豆蔻酰基转移酶（CaNMT）进行了分子对接研究。
关键词: 硅胶硫酸(SSA)；多组分反应（MCRs）；不对称芳基硫醚类化合物；分子对接；抗真菌活性
中图分类号：R914.4 文献标识码：A 文章编号：0258-3283（2017）
Synthesis, Antifungal Activity and Molecular Docking of Unsymmetrical Aryl Sulfides ZHONG Yi-fan, HAN Xiao-yan, LI Sheng-bin, QI Hui, ZHOU Zeng-hui, SONG Ya-li * (Key Laboratory of Pharmaceutical Quality Control of Hebei Province, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China), Huaxue Shiji, 2017, 39(6)
Abstract: 3-Hydroxy-5, 5-dimethyl-2-(phenyl(thiophenyl)methyl)-cyclohex-2-enone was synthesized via multicomponent reaction from thiophenol, aromatic aldehyde and 5, 5-dimethyl-1, 3-cyclohexanedione catalyzed by silica sulfuric acid(SSA). It was determined the optimum condition, such as the amount of catalyst, temperature and molar ratio of reaction reagents. The structures of objective compounds were confirmed by 1HNMR, 13CNMR, IR and HRMS. Bioassay showed that some compounds had moderate antifungal activity against C. neoformans and C. albicas. The molecular docking method was used to investigate the interaction mode of compound 4c and the N-myristoyltransferase from C. albicans（CaNMT）.
Key words: silica sulfuric acid (SSA); multicomponent reactions (MCRs); unsymmetrical aryl sulfide; molecular docking; antifungal activity
离子液体-TiO2体系选择性催化降解染料废水的研究
路鑫，辛炳炜*，冯立顺，韩海港，孟云菲，李明霞
(德州学院 山东高校配位化学与功能材料重点实验室，山东 德州 253023)
摘要：将离子液体和TiO2 P25纳米颗粒物理掺杂，构建了具有选择性降解功能的离子液体-TiO2复合光催化体系，实现了染料废水的选择性降解。研究发现，离子液体的加入能够提高TiO2对阴离子染料的降解效率，抑制阳离子染料的降解。通过优化离子液体的结构、用量等因素，筛选出了最佳复合体系[C10mim](CF3SO2)2N-TiO2 P25(物质的量比为20︰1)，紫外光照射下，20 min即可将10.0 mg/L甲基橙溶液几乎脱色完全，而对阳离子染料的降解几乎完全抑制。该体系可以选择性地降解染料废水中的某一组分，简化阴阳染料的分离和回收。
关键词：离子液体；二氧化钛；阴离子染料；阳离子染料
中图分类号：O643.3 文献标识码：A 文章编号：0258-3283（2017）
Selectively Photocatalytic Performance of Ionic Liquid-TiO2 Mixture to Dye Waste-water LU Xin, XIN Bing-wei*, FENG Li-shun, HAN Hai-gang, MENG Yun-fei, LI Ming-xia (Key Laboratory of Coordination Chemistry and Functional Materials in Universities of Shandong, Dezhou University, Dezhou 253023, China), Huaxue Shiji, 2017, 39(6)
Abstract: Ionic liquid-TiO2 mixing system was constructed by physical mixing ionic liquid and P25TiO2. The result suggested that ionic liquid could improve the decolorization rate of anionic dye, such as methyl orange, while restrain the decolorization of cationic dye. The structure and amount of ionic liquids were optimized, and found that [C10mim]Tf2N-TiO2 P25 with mole ratio 20 : 1 was the ideal system with the promising photocatalytic efficiency. It could degrade methyl orange to almost colourless after being illuminated by ultraviolet light for 20 min, whereas kept the cationic dye unfading. Ionic liquid-TiO2 mixture could simplify the species of dye waste-water, benefitting the purifition and reused.
Key words: ionic liquid; titanium dioxide; cationic dye; anionic dye
双活性中心抗菌剂磷钼钒杂多酸季铵盐的抑菌性能研究
尹彦冰*，王会淞，裴笠舟，王晓丹，宫晶
(齐齐哈尔大学 化学与化学工程学院，黑龙江 齐齐哈尔 161006)
摘要：采用水热法制备了含有不同钒原子数的Keggin型磷钼钒杂多酸季铵盐PMo12-xVxO40-TBAB (x = 1 ～ 4，TBAB为四丁基溴化铵)，选用大肠杆菌、金黄色葡萄球菌等4种菌种进行了抑菌性能测试。结果表明，合成的4种抗菌剂对大肠杆菌等菌种均有不同程度的抑菌效果，并且随着抗菌剂中钒原子数的增加，抑菌效果逐渐增强，是TBAB的1 ～ 2倍，其中PMo8V4-TBAB对大肠杆菌的抑菌效果最好。
关键词：双活性中心；抗菌剂；磷钼钒杂多酸季铵盐；抑菌性能
中图分类号：O614.51 文献标识码：A 文章编号：0258-3283（2017）
Antibacterial Performance of Double Active Central Antibacterial Reagent Molybdovanadophosphoric Heteropoly Acid Quaternary Ammonium YIN Yan-bing*, WANG Hui-song, PEI Li-zhou, WANG Xiao-dan, GONG Jing (College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, China), Huaxue Shiji, 2017, 39(6)
Abstract: The Keggin type molybdovanadophosphoric heteropoly acid quaternary ammonium PMo12-xVxO40-TBAB（x= 1 ～ 4, TBAB was tetrabutyl ammonium bromide) were synthesized via the hydrothermal method. Antibacterial performance of escherichia coli, staphylococcus aureus and other strains were investigated. The results show that the four antimicrobial agents are armed with different bacteriostatic effects to escherichia coli and other bacterium. With the increasing numbers of vanadium atoms in the agents, the antibacterial effects are improved gradually, which is one or two times of TBAB, in which the effect of PMo8V4-TBAB to Escherichia coli is the best.
Key words: double active centre; antibacterial reagent; molybdovanadophosphoric heteropoly acid quaternary ammonium; antibacterial performance
一种磺胺对甲氧嘧啶钴(II)配合物的合成、晶体结构及与DNA的作用研究
张运良1，封芬1，曾冰梅1，欧阳淼2，傅春燕1，孙双姣*1
（1. 邵阳学院 药学系，湖南 邵阳 422000；2. 河池学院 化学与生命科学系，广西 宜州 546300)
摘要：以磺胺对甲氧基嘧啶为配体，合成了一个新的钴配合物[Co(L)2(H2O)2]·2CH3OH（H-L=磺胺对甲氧嘧啶）。采用元素分析、红外光谱、质谱和X-射线单晶衍射进行结构表征。配合物属于单斜晶系，空间群为P21/c，中心金属钴与来自两个磺胺对甲氧嘧啶的磺酰胺氮、嘧啶氮及两个水分子形成六配位八面体稍变形配位构型。粘度和电泳实验表明，配合物与DNA具有一定的插入作用。
关键词：磺胺对甲氧基嘧啶；钴配合物；晶体结构；DNA
中图分类号：O626 文献标识码： A 文章编号：0258-3283（2017）文章编号：0258-3283（2017）
Synthesis, Crystal Structure, DNA Interaction of Co(II) Complex with 4-Amino-N-(5-methoxy-2-pyrmidiny)benzenesulfonamide ZHANG Yun-liang1, FENG Fen1, ZENG Bing-mei1, OUYANG Miao2, FU Chun-yan1, SUN Shuang-jiao*1（1. Department of Pharmacy, Shaoyang College, Shaoyang 422000, China; 2. School of Chemistry and Bioengineering, Hechi University, Yizhou 546300, China), Huaxue Shiji, 2017, 39(6)
Abstract: A new Co(II) complex, [Co(L)2(H2O)2]·2CH3OH (1)(H-L = 4-amino-N-(5-methoxy-2-pyrmidiny)benzenesulfonamide), was synthesized and fully confirmed by elemental analysis, IR and single crystal X-ray diffraction analysis. The results show that 1crystallized in a Monoclinicsystem with space group P21/c. .The Co(II) is six-coordinated by two L via two sulfonamide N atoms, two pyridazine N atoms, as well as two O atoms from two water, forming a slightly distorted octahedral geometry. The viscosity measurement and gel electrophoresis test indicated that complex can bind with DNA by intercalative binding mode.
Key words: 4-amino-N-(5-methoxy-2-pyrmidiny)benzenesulfonamide; cobalt(II) complex; crystal structure; DNA interaction
N-乙酰-L-酪氨酸甲酯偶氮衍生物的合成及紫外可见光谱学性质
汤军1，汪大巍1，操燕明1，高小红1，杜松云1，吕早生*2
(1. 武汉华夏理工学院 生物与制药工程学院，湖北 武汉 430223；
2. 武汉科技大学 化学工程与技术学院，湖北 武汉 430081)
摘要：以N-乙酰-L-酪氨酸甲酯为原料，合成了6个新型的偶氮衍生物，通过IR、1HNMR、13CNMR、EI-MS和元素分析进行了表征。考察了所合成化合物的偶氮式-腙式互变异构以及溶剂和pH对紫外可见光谱的影响。结果表明，溶质-溶剂相互作用会影响化合物在不同溶剂的λmax发生微小的变化，分子内和分子间氢键的作用影响较大。溶液pH会直接影响偶氮式和腙式的平衡构成，随着pH的增加，偶氮式在偶氮式-腙式互变异构平衡中的比例逐渐降低。这些偶氮化合物有望成为一类潜在的pH指示剂。
关键词：N-乙酰-L-酪氨酸甲酯偶氮衍生物；偶氮-腙互变异构；紫外可见光谱
中图分类号：O625.65 文献标识码：A 文章编号：0258-3283（2017）
Synthesis and UV-Vis Spectrum of N-Acetyl-L-tyrosine Methyl Ester Azo Derivatives TANG Jun1, WANG Da-wei1, CAO Yan-ming1, GAO Xiao-hong1, DU Song-yun1, LV Zao-sheng*2(1. Department of Biological and Pharmacy Engineering, Wuhan Huaxia University of Technology, Wuhan 430223, China; 2. School of Chemical Engineering and Technology, Wuhan University of Science and Technology, Wuhan 430081, China), Huaxue Shiji, 2017, 39(6)
Abstract: Six new azo compounds were synthesized, N-acetyl-L-tyrosine methyl ester as raw material. The structures of the new azo compounds were confirmed by IR and 1HNMR. The effects of various solvent and pH values upon the absorption spectra of the azo compounds were tested to investigate the azo-hydrazonetautomerizm phenomena. The results showed that the solute-solvent interactions in different solvents can affect minor changes of λmax in the compounds, the role of intra molecular and intermolecular hydrogen bonds plays an important role. The proportion of azo tautomer in azo-hydrazonetaotomerizm equilibrium is decreased with the increasing of pH. These new azo compounds could potentially be used as pH indicators.
Key words: N-acetyl-L-tyroaine methyl ester azo compounds; azo-hydrazonetautomerizm; UV-Vis spectrum
PFOA和PFOS去除技术研究进展
杨海，令狐文生*
（绍兴文理学院 化学化工学院，浙江 绍兴 312000）
摘要：全氟辛酸（PFOA）和全氟辛烷磺酸（PFOS）是一类新型难降解的持久性污染物。由于在环境中有很高的生物蓄积性、多种毒性和稳定持久性，近年来PFOA/PFOS去除技术的相关研究被国内外学者广泛关注和重视。针对PFOA/PFOS在环境中的污染状况及各种去除技术的研究进展进行了综述，并对当前各种去除技术存在的问题进行了分析和探讨。
关键词：全氟辛酸；全氟辛烷磺酸；环境污染；去除技术
中图分类号：O658 文献标识码：A 文章编号：0258-3283（2017）
Progress on Removal Methods of PFOA and PFOS Pollutants YANG Hai, LINGHU Wen-sheng* (College Chemistry & Chemical Engineering, Shaoxing University, Shaoxing 312000, China), Huaxue Shiji, 2017, 39(6)
Abstract: Perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) are a new type of refractory total fluoride compound in environmental pollution. Recently, due to the highly biological accumulation, multiple toxicity, and stable persistence in the environment, the related researches of PFOA/PFOS removal technology have been widely concerned and valued by domestic and foreign scholars. In this work, the pollution of PFOA/PFOS and various removal technologies are developed. Then the problems in these technologies were discussed.
Key words：perfluorooctanoate; perfluorooctane sulfonate; environmental pollution; removal technology
1H-吲唑的合成研究进展
孙明娜*，张建业，王声，余碧丹，符弼妮，张丹欢
（广州医科大学 药学院，广东 广州 511436）
摘要：吲唑是一类重要的杂环化合物及合成中间体，具有广泛的生物学活性（如抗炎、抗肿瘤、抗氧化、抗病毒、抗菌等），是药物分子中常见的优势骨架，也广泛应用于除草剂、染料等。目前，已有多种方法合成吲唑，特别是1H-吲唑，重点围绕不同的起始原料，综述了1H-吲唑类化合物的典型合成方法。
关键词：吲唑；合成；杂环化合物；起始原料
中图分类号：O626.2 文献标识码：A 文章编号：0258-3283（2017）
Progress of Synthesis of 1H-Indazoles SUN Ming-na*, ZHANG Jian-ye, WANG Sheng, YU Bi-dan, FU Bi-ni, ZHANG Dan-huan(School of Pharmaceutical Sciences, Guangzhou Medical University, Guangzhou 511436, China), Huaxue Shiji, 2017, 39(6)
Abstract: Indazoles is an important class of heterocyclic compounds and synthetic intermediates having a wide range of biological and pharmaceutical activities, as anti-inflammatory, anti-tumor, anti-oxidant, anti-viral, anti-bacterial. There is enormous potential in the synthesis of indazoles to be used as building blocks for the next generation of pharmaceuticals, as well as herbicides and dyes. Various synthetic routes have been reported for indazoles, especially 1H-indazoles. The present review focuses on typical routs of their synthesis from diverse materials.
Key words: indazoles; synthesis; heterocyclic compounds; starting materials
甘脲及其衍生物的研究进展
郑志花*，王建龙，马文兵
（中北大学 化工与环境学院，山西 太原 030051）
摘要：甘脲自1877年合成以来，随后制备了一系列的甘脲及其衍生物，在涂料、炸药、水处理、电子器材、超分子识别及药物、农药缓释、分子催化等方面具有广泛的用途。简要介绍迄今为止甘脲及其衍生物的制备方法及应用方面的研究进展。
关键词：甘脲；乙二醛；脲；合成；应用
中图分类号：TQ630；TJ55；O631；O626 文献识别码：A 文章编号：0258-3283（2017）
Progress of Glycoluril and Derivatives ZHENG Zhi-hua*, WANG Jian-long, MA Wen-bin（School of Chemical Engineering and Environment, North University of China, Taiyuan 030051, China）, Huaxue Shiji, 2017, 39(6)
Abstract: Glycoluril was synthesized since 1877, subsequently, a series of glycoluril and its derivatives have been prepared, They can been widely used in many fields, such as coating, powder, water treatment, electronic equipment, super molecular recognition and assembly, self-assembly, the release of drug and pesticide, molecular catalysis, and so on. In this review, the recent research results about the preparation methods and applications of glycoluril and its derivatives are briefly introduced.
Key words: glycoluril; glyoxal; urea; synthesis; application
咪唑离子液体为背景HPCE测定血清中头孢药物
李敏*1，夏爱清1，乔卫叶1，成丽苹1，王秀玲1，孙杰2
（1. 邢台学院 化学工程与生物技术学院，河北 邢台 054001；
2. 江苏力维检测科技有限公司，江苏 无锡 214000）
摘要：建立了以[Bmim][BF4]离子液体作为背景电解质，高效毛细管电泳同时测定血清中头孢噻肟(CTX)、头孢唑啉(CFZ)、头孢曲松(CRO)和头孢米诺（CMN）这4种头孢类药物的方法。将头孢拉定(RAD)作为内标，考察了背景电解质的浓度、分离电压、溶液pH、进样时间对分离度的影响。结果发现，背景电解质浓度为30 mmol/L [Bmim][BF4](pH 10.5)、分离电压为15 kV、进样时间为10 s、检测波长为250 nm，CTX、CFZ、CRO和CMN在9 min内能得到有效地分离，在0.5 ～ 100.0 mg/L范围内有良好的线性关系（r > 0.999），检出限分别为0.61、0.56、0.46和0.79 mg/L，定量限分别为2.05、1.90、1.56和2.65 mg/L，精密度（RSD）< 3.2%。该方法用于血清中头孢药物的分析，回收率为97.16% ～ 101.40%。离子液体经CH2Cl2萃取回收，回收率达85%以上。
关键词：HPCE；电解质；离子液体；头孢抗生素；血清
中图分类号：O652.7 文献标识码：A 文章编号：0258-3283（2017）
Simultaneous Determination of Four Cephalosporins in Serum by High Performance Capillary Electrophoresis with Ionic Liquid as Background LI Min*1, XIA Ai-qing1, Qiao Wei-ye1, CHENG Li-ping1, WANG Xiu-ling1, SUN Jie2（1. College of Chemical Engineering and Biotechnology, Xing Tai University, Xingtai 054001, China; 2. Jiangsu Levei Testing Company Limited, Wuxi 214000, China）, Huaxue Shiji, 2017, 39(6)
Abstract: A capillary electrophoresis method has been developed for the simultaneous determination of four cephalosporins (cefotaxime(CTX), cefazolin(CFZ), ceftriaxone(CRO) and cefminox(CMN)) with ionic liquid as background in serum. Using cefradine(RAD) as internal standard, the influence of the electrophoretic parameters(concentration of background electrolyte, voltage, pH values and injection time) on the separation was investigated. The best result was obtained using 30 mmol/L [Bmim][BF4] (pH 10.5) as background, at 15 kV, the injection time of 10 s, UV detection at 250 nm. The four cephalosporins were effectively separated in less than 9 minutes and good linear relationship (r>0.999) were obtained in the 0.5 ~ 100.0 mg/L range. The detection limits of four cephalosporins were 0.61, 0.56, 0.46 and 0.79 mg/L, respectively. The limits of quantification were 2.05, 1.90, 1.56 and 2.65 mg/L respectively and RSD was <3.2%. The method was applied to the determination of the cephalosporins in serum and recovery was in the range from 97.16% ~ 101.40%. Ionic liquids was extracted by CH2Cl2 and recovery was more than 85%.
Key words: HPCE; electrolyte; ionic liquid; cephalosporins; serum
智能手机拍摄数码比色法测定水样中痕量肼
丁宗庆*，周向宇，刘光东
（汉江师范学院 生物化学与环境工程系，湖北 十堰 442000）
摘要：建立了智能手机拍摄数码比色法测定水样中痕量肼的新方法，水样中肼和对二甲氨基苯甲醛显色后用手机直接拍摄溶液图像，用Photoshop软件采集图像中显色液蓝色通道的亮度值ΔB，溶液中肼的质量浓度与ΔB值呈线性关系。方法的线性范围为0.008 ～ 0.320 mg/L (R ＝ 0.9997)，检出限为0.002 mg/L，实际样品的加标回收率为97.5% ～ 104%，相对标准偏差为2.3% ～ 3.8%。方法不使用专业仪器设备，测定结果与分光光度法吻合，操作便捷、成本低，可实现现场的快速测定。
关键词：智能手机；数码比色；肼；水样
中图分类号：O661.1 文献标识码：A 文章编号：0258-3283（2017）
Determination of Trace Hydrazine in Water Samples by Smartphone Shooting Digital Colorimetry DING Zong-qing*, ZHOU Xiang-yu, LIU Guang-dong (Department of Biological, Chemical & Environmental Engineering, Hanjiang Normal University, Shiyan 442000, China)
Abstract: A new method for the determination of trace hydrazine by smartphone shooting digital colorimetry was proposed. The picture of the hydrazine solution with p-dimethylaminobenzaldehyde from smartphone shooting was imported into the software Photoshop to obtain the brightness value ΔB of blue channels. The experimental data showed that ΔB value is linearly correlated with the concentration of hydrazine in solution. A good linear relationship was obtained in the range of 0.008～0.320 mg/L (R = 0.9997), the detection limits of 0.002 mg/L. The recoveries fell in the range from 97.5% to 104% and the relative standard deviations were between 2.3% and 3.8%. The method can be applied in the field detection without the professional instruments and its result is in agreement with that of spectrophotometric method. It is simple, rapid and economical.
Key words: digital colorimetry; smartphone; hydrazine; water sample
ATR-FTIR结合判别分析法快速鉴别
天然柠檬风味精油种类
陈梓云*，黄云，梁焱红，阮韵丹
（嘉应学院 化学与环境学院，广东 梅州 514015）
摘要：以5种山苍子精油、2种柠檬草精油为研究对象，采用ATR-FTIR结合判别分析法建立了几类天然柠檬风味精油的识别模型。模型清晰地将样品分成了3大类：低浓度柠檬醛精油、高浓度柠檬醛精油、烯烃类（柠檬烯及长叶烯）精油。利用模型可以简便、快速地鉴别不同类型的天然柠檬风味精油，为天然柠檬风味精油的快速鉴别提供了一种新的方法。
关键词：红外光谱法；判别分析；鉴别；柠檬风味精油
中图分类号：O657.33 文献标识码：A 文章编号：0258-3283(2017)
Identification of Natural Lemon-flavored Oil by Infrared Spectroscopy Combined with Discriminant Analysis CHEN Zi-yun*, HUANG Yun, LIANG Yan-hong, RUAN Yun-dan (School of Chemistry and Environment, Jiaying University, Meizhou 514015, China), Huaxue Shiji, 2017, 39(6)
Abstract：Taking seven kinds of different quality of natural lemon flavor oil (five kinds of cubeba essential oil, two kinds of lemongrass essential oil) as the object, the recognition natural lemon flavor oil model was established using ATR-FTIR combined with discriminant analysis. The samples were clearly divided into three categories by model: low concentrations of citral oil, high concentrations of citral oil, limonene and longifolene oil. The model can be easily and quickly identify different quality natural lemon flavor oils. It provides a new method for the identification of natural lemon flavor oil.
Key words：ATR-FTIR; discriminant analysis; identification; natural lemon-flavored oil
阿魏酸哌嗪在铁氰化钾体系中的显色反应研究
潘自红*，王亚波，曹云丽，杜娴，张彬艳
(平顶山学院 化学与环境工程学院，河南 平顶山 467000)
摘要：研究了阿魏酸哌嗪在铁氰化钾体系中氧化还原反应及显色反应，建立了一种快速、简便测定阿魏酸哌嗪的分光光度法。实验利用阿魏酸哌嗪的还原性，可将Fe(Ⅲ)还原，生成的Fe(Ⅱ)与K3[Fe(CN)6]反应生成蓝色化合物，再以其最大吸收波长755 nm处进行测定体系的吸光度，计算阿魏酸哌嗪的含量，探讨其反应机理及反应的动力学性质。阿魏酸哌嗪的浓度在0.08 ~ 17.183 mg/L范围内与吸光度呈良好的线性关系，对其进行作图得线性回归方程为A = 0.02937 + 0.14147 c (mg/L，r = 0.9991)，表观摩尔吸光系数ε为6.71×104 L/(mol•cm)，方法的检出限和精密度的RSD分别为0.0395 mg/L和0.76%。将本方法应用于阿魏酸哌嗪片中阿魏酸哌嗪含量的测定，加标后平均回收率为99.7%。
关键词：阿魏酸哌嗪；分光光度法；氯化铁；铁氰化钾
中图分类号：O657.32 文献标识码：A 文章编号：0258-3283（2017）
Chromogenic Reaction of Piperazine Ferulate in the System of Potassium Ferricyanide PAN Zi-hong*, WANG Ya-bo, CAO Yun-li, DU Xian, ZHANG Bin-yan (College of Chemistry and Environmental Engineering, Pingdingshan University, Pingdingshan 467000, China)
Abstract：The redox reaction and chromogenic reaction of piperazine ferulate in the system of potassium ferricyanide have beeninvestigated by spectrophotometric method. A simple and rapid method for the determination of piperazine ferulate was established. It was based on the fact that Fe(Ⅱ) generated from Fe(Ⅲ) using the reducibility of piperazine ferulate could react with potassium ferricyanide to form the blue compound. Then, the absorbance of the compound was determined at the maximal absorption wavelength of 755 nm and the content of piperazine ferulate was calculated. The reaction mechanism and kinetic property were elucidated intensively. Beer’s law was obeyed in the range of 0.08～17.183 mg/L of piperazine ferulate. The equation of linear regression equation was A = 0.02937 + 0.14147 c (mg/L) with a correlation coefficient of 0.9991 and the apparent molar absorption coefficient of 6.71×104 L/(mol•cm). The detection limit was 0.0395 mg/L, while RSD was 0.76% . This proposed method has been applied to the determination of piperazine ferulate in tablets, with average recovery rate of 99.7%.
Key words: Piperazine ferulate; Spectrophotometry; Fe(Ⅲ); potassium ferricyanide
有机相阴离子交换SPE-UPLC-UV法快速测定
食用植物油中抗氧化剂TBHQ和BHA
刘萍*，李晓，章思倩，陶玉佩
（台州科技职业学院 农业与生物工程学院，浙江 台州 318020）
摘要：建立了基于有机相阴离子交换SPE前处理的UPLC-UV法快速测定食用植物油中抗氧化剂TBHQ和BHA。食用植物油样品用正己烷稀释后，直接上样至Oasis MAX聚合物材质阴离子交换SPE柱中进行净化，用正庚烷淋洗去除甘油酯成分，用0.5%甲酸四氢呋喃溶液洗脱。以纯水和甲醇为流动相，TBHQ和BHA在Eclipse Plus C18上和梯度洗脱条件下3.4 min内达到基线分离；检测波长为290 nm；进样量为1 μL。TBHQ和BHA在5 ~ 200 mg/L范围内线性关系良好（r≥0.99995）；在10、50、200 mg/kg这3个水平的加标回收率为91.5% ~ 104%，相对标准偏差为1.2% ~ 4.4%。方法定量限为0.5 mg/kg。与已有方法相比，该方法样品前处理更简便快速、色谱分离时间短、结果准确，可广泛应用于食用植物油样品中TBHQ和BHA等抗氧化剂的快速检测。
关键词：有机相阴离子交换；SPE；UPLC-UV；食用植物油；抗氧化剂；TBHQ；BHA
中图分类号：O657.7 文献标识码：A 文章编号：0258-3283（2017）
A Rapid UPLC-UV Method for Simultaneous Determination of Antioxidants TBHQ and BHA in Edible Vegetable Oils Based on Organic Phase Anion Exchange SPE LIU Ping*, LI Xiao, ZHANG Si-qian, TAO Yu-pei（ , Taizhou Vocational College of Science & Technology, Taizhou 318020, China）, Huaxue Shiji, 2017, 39(6)
Abstract: A rapid UPLC-UV method for simultaneous determination of antioxidants TBHQ and BHA in edible vegetable oils was developed based on organic phase anion exchange SPE. Vegetable oils were directly diluted with n-hexane, and then loaded into Oasis MAX cartridges for purification, n-heptane was adopted to remove glycerides residues in the cartridge bed. TBHQ and BHA were eluted into a glass tube with 0.5% formic acid tetrahydrofuran solution. The eluted sample solution was mixed thoroughly, and then filtered into the sampling bottles with a PFTE syringe filter for UPLC analysis. The pure water and methanol were selected as the mobile phase, TBHQ and BHA were separated completely within 3.4 min with Eclipse Plus C18 UPLC column in a gradient elution mode. The wavelength of detector was set at 290 nm. The injection volume was 1 μL. The linearity of the method was good with ≥0.99995 over the concentration range from 5 to 200 mg/L. The recoveries for TBHQ and BHA were between 91.5.6% and 104% with the relative standard deviation between 1.2% and 4.6% at 10, 50 or 200 mg/kg levels. The limits of quantification were 0.5 mg/kg for both TBHQ and BHA. The method shows the more rapid and easier sample pretreatment operations, much shorter chromatographic separation time, good recoveries and accuracies. The method can be widely applied in rapid analysis of antioxidants like TBHQ and BHA in edible vegetable oils
Key words：UPLC-UV; antioxidants; TBHQ; BHA; edible vegetable oils; organic phase anion exchange; SPE
Al3+荧光探针的合成及识别性能研究
姜秀娟*a，朱荣贵b，王寿峰a，陈依依a，付大友a，林莉a
（四川理工学院 a. 分析测试中心，b. 生物工程学院，四川 自贡 643000）
摘要：以2-羟基-1-萘甲醛和邻苯二胺为原料，通过席夫碱反应合成了一个Al3+荧光探针。采用紫外-可见和荧光光谱法研究了探针在乙腈溶液中对金属离子的识别能力。实验结果表明，该探针在乙腈及其水溶液中可以有效快速地检测Al3+。通过荧光滴定曲线、Job′s曲线和Benesi-Hildebrand曲线，得出探针分子与Al3+的配合比和配合常数分别为2 : 1和2.65×105，并测得Al3+的最低检出限为1.85×10−8 mol/L。
关键词：荧光探针；萘；Al3+识别
中图分类号：O657.3 文献标识码：A 文章编号：0258-3283（2017）
Synthesis and Recognition Properties of a Fluorescence Sensor for Al3+ Based on Naphthalene JIANG Xiu-juan*a, ZHU Rong-guib, WANG Shou-fenga, CHEN Yi-yia, FU Da-youa, LIN Lia (a. Analytical and Testing Center, b. College of Bioengineering, Sichuan University of Science and Engineering, Zigong 643000, China), Huaxue Shiji, 2017, 39(6)
Abstract: A fluorescent probe for Al3+ was synthszied by the Schiff-base reaction of 2-hydroxy-1-naphthaldehyde and o-phenylene.The recognition properties of the probe for metal ions have been investigated by the UV-Vis and fluorescence spectrophotometry in acetonitrile solution. The results showed that the probe could effectively and quickly detect Al3+ in acetonitrile and its aqueous solution. The complexation ratio and the binding constant of the probe L with Al3+ by the fluorescence titration curve, Job′s plot and Benesi-Hildebrand plot were 2 : 1 and 2.65×105, respectively. The detection limit for Al3+ was 1.85×10−8 mol/L.
Key words: fluorescent probe; naphthalene; Al3+recognition
丙酮与重水氢-氘交换反应催化剂的考察研究[1]
王雪婷，王伟，杜晓宁*，卢伟京，侯捷，雷雯，岳韩笑，徐建飞
（上海化工研究院 上海稳定性同位素工程技术研究中心，上海 200062）
摘要：为丙酮与重水氢-氘交换的基础研究，考察了丙酮与重水在不同催化剂存在下的一次交换效果，并利用单因素实验，考察了n(重水) ∶n(丙酮) = 12.5∶1固定条件下，催化剂的用量、反应温度和反应时间对丙酮氢-氘交换（H-D交换）反应的影响。结果表明，产物氘代丙酮的氘同位素丰度随着以上变量增加先增加后平衡，平衡条件为碳酸钠添加量0.0159 mol/mol、反应温度45 ℃、平衡时间3 h，交换后丙酮的氘原子同位素丰度达到80.53 atom%D。
关键词：氘代丙酮；H-D交换；催化剂；稳定同位素
中图分类号：O69；O62；TQ 文献识别码：A 文章编号：0258-3283（2017）
H-D Exchange Catalyst of Acetone with Deuterium Oxide WANG Xue-ting, WANG Wei, DU Xiao-ning*, LU Wei-jing, HOU Jie, LEI Wen, YUE Han-xiao, XU Jian-fei (Shanghai Research Center of Stable Isotope Engineering Technology, Shanghai Research Institute of Chemical Industry, Shanghai 200062, China), Huaxue Shiji, 2017, 39(6)
Abstract: The basic conditions of hydrogen-deuterium exchange (H-D exchange) reactions of deuterium oxide with acetone were inspected in this work. The effects of kinds of acidic and alkaline catalyst and amount, reaction temperature, reaction time were investigated for deuterium oxide with acetone at a constant proportion of 12.5∶1. Among them, sodium carbonate was the best one. The atom of the isotope abundance of acetone deuterium was 80.53atom%D at the suitable H-D exchange reaction condition, sodium carbonate dosage of 0.0159 mol/mol, 45 oC for 3 hours.
Key words: deuterium labeled acetone; H-D exchange; catalysts; stable isotope
基于含铜簇配位聚合物的制备及晶体结构
王俊*1，吕平2
（1. 中山职业技术学院 信息工程学院，广东 中山 528404；
（2. 天津职业大学 生物与环境工程学院，天津 300402）
摘要：通过席夫碱配体2-羟基-3-甲氧基-苯甲醛缩烟酰肼(IAH)和碘化亚铜在溶剂热条件下得到新型的铜(I)配位聚合物[(Cu2I2)L]n。通过红外光谱和热重分析等方法对该配合物进行了表征，并测定了它的单晶结构，配合物属三斜晶系，空间群P-1，a = 7.9988(8) Å，b = 12.6423(12) Å，c = 17.9197(17) Å，α = 89.528(2)º，β = 89.528(2)º，γ = 73.6880(10)º，V = 1738.9(3) Å3，Z = 2。
关键词：铜簇；配位聚合物；合成；晶体结构
中图分类号：O72 文献标识码：A 文章编号：0258-3283（2017）
Synthesis and Crystal Structure of Copper Cluster Based Coordination Polymer WANG Jun*1, LV Ping2(1. , Zhongshan Polytechnic, Zhongshan 528404, China; 2. School of Biological and Environmental Engineering, Tanjin Vocational Institute, Tianjin 300402, China), Huaxue Shiji, 2017, 39(6)
Abstract: A novel coordination polymer [(Cu2I2)L]n, was synthesized by Schiff base ligand (2-hydroxy-3-methoxy-benzylidene)-hydrazide (IAH), isonicotinic acid and CuI under solvothermal condition. The title compound was characterized by elemental analysis, IR and thermogravimetry analysis. The structure of the compound [(Cu2I2)L]n was confirmed by X-ray single crystal diffraction analysis. The results showed that the crystallize is in triclinic space group P-1 with a = 7.9988(8) Å, b = 12.6423(12) Å, c = 17.9197(17) Å, α = 89.528(2)º, β = 89.528(2)º, γ = 73.6880(10)º, V = 1738.9(3) Å3, Z = 2。
Key words: copper cluster; coordination polymer; synthesis; crystal structure
2-丁基癸二酸的合成及其电化学性能研究
刘长春，闻立新，程进，刘承先*，戴溢，郭程
（常州工程职业技术学院化学与材料工程学院，江苏常州213164）
摘要: 以正丁基丙二酸二乙酯和8-溴辛酸乙酯为原料，经过烷基化、水解和脱羧等步骤制备2-丁基癸二酸，收率为87.8%，通过1HNMR、13CNMR、IR和元素分析对其结构进行了表征。并用该化合物在乙二醇中与氨气反应制备成电解质溶液，溶液的电导率为2.60mS/cm（30℃），闪火电压为455V（85℃），氧化效率为1.65(2mA)，测试性能优于现有产品。
关键词: 2-丁基癸二酸；高压铝电解电容器；电解液；闪火电压
中图分类号:O623.6 文献标识码:A 文章编号:0258-3283（2017）
Synthesis and Electronic Chemical Performance of 2-Butyldecanedioic Acid LIU Chang-chun, WEN Li-xin, CHENG Jin, LIU Cheng-xian*, DAI Yi, GUO Cheng (School of Chemistry and Materials Engineering, Changzhou Institute of Engineering Technology, Changzhou 213164)
Abstract: 2-Butyldecanedioic acid was synthesized by using diethyl 2-butylmalonate and ethyl 8-bromoocatanoate via alkylation, hydrolysis and dicarboxylicreactions with the total yield of 87.8%, which was confirmed by 1HNMR, 13CNMR, IR and elemental analyses. After reacting with ammonia, 2-butyldecanedioic acid was used to prepare an electrolyte with the conductivity of 2.60 mS/cm (30 ℃), the spark voltage of 455 V (85 ℃), and a high oxidizing efficiency of 1.65(2 mA)，which performance was superior to commercially available products.
Key words: 2-butyldecanedioic acid; high-voltage aluminum electrolytic capacitor; electrolyte; spark voltage
DMAB显现纸张表面潜在手印应用研究
赵雅彬*1，罗军2，罗亚平1，郭威1，江沅龙1
（1. 中国人民公安大学 刑事科学技术学院，北京 100038；
2. 江苏省海安县公安局 刑事科学技术室，江苏 南通 226600）
摘要：纸张类客体是案件现场常见的一类检材，其表面潜在手印的显现在物证检验鉴定过程中具有重要的意义。利用氨基酸敏感试剂N, N-二甲基-4-氨基苯甲醛（DMAB）对纸张表面潜在手印进行显现研究，结果表明，当浓度为0.4%时，DMAB对纸张表面潜在手印有很好的显现效果，显现手印在490 nm光源照射时，橙色护目镜下可观察到黄色荧光。该方法显现灵敏度高、显出手印纹线清晰、与背景反差较大，对于遗留30 d的陈旧性手印仍然具有良好的显现效果。
关键词：DMAB；纸张表面；潜在手印；显现；物证鉴定
中图分类号：DF794.1 文献标识码：A 文章编号：0258-3283（2017）
Development of Latent Fingermarks on Papers by DMAB ZHAO Ya-bin*1, LUO Jun2, LUO Ya-ping1, GUO Wei1, JIANG Yuan-long1(1. School of Forensic Science, People′s Public Security University of China, Beijing 100038, China;2. Criminal Science and Technology Institute, Haian Municipal Public Security Bureau, Jiangsu 226600, China), Huaxue Shiji, 2017, 39(6)
Abstract: Paper is one of the most common substrates in crime scenes, the detection of fingermarks on papers is crucial in the investigation of crime scenes and evidence identification. In this work, experiments were conducted by amino acid sensitive reagent DMAB. The new method reported here exhibited good selectivity and sensitivity in the detection of fingermarks in various paper substrates. Moreover, the results showed that remarkable prints have been observed in 0.4% (m/v) formulation under 490 nm illumination, with orange goggles, even for the fingermarks aged for 30 d, it still showed good ridges clarity and excellent contrast.
Key words: DMAB; paper substrates; latent fingermarks; development; evidence identification
减压蒸馏辅助熔融结晶分离技术制备高纯二甲基亚砜
顾金凤，郭建国*，陈浩云
（国药集团化学试剂有限公司，上海 200002）
摘要：二甲基亚砜（DMSO）是一种非质子极性溶剂，由于它对化学反应具有特殊的溶媒效应以及对许多物质的溶解特性，因此被称为“万能溶剂”。目前，在石油、化工、医药、电子、合成纤维、塑料、印染等许多化工领域具有广泛的应用。采用减压蒸馏辅助熔融结晶分离技术制备二甲基亚砜。该方法具有操作简便、环境友好、纯化效率高等优点，为规模生产提供了一种新的手段。
关键词：二甲基亚砜；氧化钙；大孔分子筛；减压蒸馏；熔融结晶
中图分类号：TQ064 文献标识码：A 文章编号：0258-3283（2017）
Vacuum Distillation Assist Melt Crystallization Separation Technology to Prepare High Purity Dimethyl Sulfoxide GU Jin-feng, GUO Jian-guo*, CHEN Hao-yun（Sinopharm Chemical Reagent Co., LTD , Shanghai 200002, China）, Huaxue Shiji, 2017, 39(6)
Abstract: Dimethyl sulfoxide (DMSO) is an aprotic polar solvent. Because it have a special solvent effect on the chemical reaction and dissolution characteristics of many substances, therefore is called the "universal solvent". At present, in petroleum, chemical, pharmaceutical, electronics, synthetic fibre, plastic, printing, dyeing, etc many fields of chemical industry has a wide range of applications. This paper adopts the vacuum distillation auxiliary melt crystallization separation technology of preparation of dimethyl sulfoxide. The method is simple, environmental friendly, high purification efficiency, provides a new means for scale production.
Key words: dimethyl sulfoxide; calcium oxide; macroporous molecular sieve; vacuum distillation melt crystallization
一种应用催化不对称硼氢化反应合成(S)-布洛芬的新方法
付伟谊1，强敏1，刘晓峰*1, 2，张隆1，万文浩1
(1. 武汉科技大学 化学与化工学院，湖北 武汉 430081；2. 浙江仙居君业药业有限公司，浙江 仙居 317300)
摘要：以4-异丁基苯乙酮为原料，发展了一条简洁的(S)-布洛芬不对称合成方法。经4步反应得到具有光学活性的(S)-布洛芬，光学纯度（e.e.）达到66%，总收率为61%，其关键步骤为一步催化不对称硼氢化1, 1-二取代末端烯烃。
关键词：[Ir(OMe)(COD)]2；膦配体；不对称硼氢化；(S)-布洛芬
中图分类号：O625.51 文献标识码：A 文章编号：0258-3283（2017）
A Novel Synthesis of S-Ibuprofen via a Catalytic Asymmetric Hydroboration FU Wei-yi1, QIANG Min1, LIU Xiao-feng*1, 2, ZHANG Long1, WAN Wen-hao 1 (1. School of Chemistry and Chemical Engineering, Wuhan University of Science and Technology, Wuhan 430081, China; 2. Zhejiang Xianju Junye Pharmaceutical Co., Ltd, Xianju 317300, China), Huaxue Shiji, 2017, 39(6)
Abstract: A concise asymmetric synthesis of S-2-(4-isobutylphenyl)propionic acid (S-ibuprofen) has been achieved in 59% overall over 4 steps with 66%(e.e.), using a catalytic asymmetric hydroboration of 1-isobutyl-4-(prop-1-en-2-yl)benzene as the key step.
Key words: [Ir(OMe)(COD)]2; phosphinooxazoline ligands; asymmetric hydroboration; (S)-ibuprofen
二甲基二氧杂环丙烷的制备及在25-羟基胆固醇合成中的应用
王建塔，陈文章，夏晶，赵平，谢珺，汤磊*
（贵州医科大学 药学院，贵州 贵阳 550004）
摘要：以胆固醇为起始原料，经酰化、溴代、二甲基二氧杂环丙烷氧化、还原等4步反应合成了25-羟基胆固醇，总收率为62.7%，其结构经过1HNMR和13CNMR鉴定。
关键词：二甲基二氧杂环丙烷；25-羟基胆固醇；合成
中图分类号：TQ282 文献标识码：A 文章编号：0258-3283（2017）
Preparation of Dimethyldioxirane and itsApplication in the Synthesis of 25-Hydroxycholesterol WANG Jian-ta, CHEN Wen-zhang, XIA Jing, ZHAO Ping, XIE Jun, TANG Lei*（School of Pharmacy, Guizhou Medical University, Guiyang 550004, China）, Huaxue Shiji, 2017, 39(6),
Abstract：Using cholestererol as starting material, 25-hydroxycholesteral has been achieved in four steps via acylation, bromanation, oxidation and reduction with a total yield of 62.7%. And the final product was confirmed by 1HNMR and 13CNMR.
Key words：dimethyldioxirane; 25-hydroxycholesterol; synthesis
固体碱催化Knoevenagel法合成阿魏酸的工艺研究
李修刚，胡仕琴，杨航周，黄启鹏，孔雷，张玲钰*
（铜仁学院 材料与化学工程学院，贵州 铜仁 554300）
摘要：以香兰素和丙二酸为原料、苯为带水剂、固体碱为催化剂、吡啶为助催化剂，经Knoevenagel反应合成了阿魏酸，经重结晶提纯得到目标化合物，并对化合物进行了结构验证。结果表明，n(香兰素)︰n (丙二酸) = 1 : 1.15，吡啶为5 wt%香兰素、固体碱催化剂为3 wt%香兰素时，反应效果最佳，阿魏酸的收率可达90%以上。
关键词：阿魏酸；Knoevenagel反应；香兰素；固体碱
中图分类号：TQ252.3 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of Ferulic Acid by Knoevenagel Method with Solid Base LI Xiu-gang, HU Shi-qin, YANG Hang-zhou, HUANG Qi-peng, KONG Lei, ZHANG Ling-yu*(College of Material and Chemical Engineering, Tongren University, Tongren 554300, China), Huaxue Shiji, 2017, 39(6)
Abstract: In this work, ferulic acid was synthesized by Knoevenagel reaction, in which vanillin and malonic acid, benzene, solid base and pyridine were used as starting materials, water-carrying agent, catalyst and co-catalyst, respectively. The product was purified by recrystallization, then the structure was confirmed. The optimal reaction conditions were as follows molar ratio of vanillin tomalonic acid was 1: 1.15, the mass rations of pyridine and solid base in vanillin were 5 wt% and 3 wt%, respectively. The yield of ferulic acid could reach above 90% by using the optimal reaction condition.
Key words: Ferulic acid; Knoevenagel reaction; Vanillin; solid base
2, 1-苯并异恶唑的合成新方法
潘涛，刘霞*，沈宏，李方雷
（江苏开放大学 环境与生态学院，江苏 南京 210036）
摘要：以硝基苯甲醛及叠氮钠为主要原料、五水硫酸铜和抗坏血酸钠为催化剂、N-甲基吡咯烷酮为溶剂（NMP），探讨溶剂种类及催化剂用量、反应温度等条件对反应的影响，“一锅法”合成苯并异恶唑。与传统方法相比，该方法具有原料廉价易得、底物适用性广、收率高及条件温和等特点。目标化合物结构经1HNMR、13CNMR、MS及元素分析等表征。
关键词：五水硫酸铜；苯并异恶唑；一锅煮；合成
中图分类号：O626 文献标识码：A 文章编号： 0258-3283（2017）
New Synthetic Method of 2, 1-Benzisoxazoles PAN Tao, LIU Xia*, SHEN Hong, LI Fang-lei (College of Environment Science and Ecology, Jiangsu Open University, Nanjing 210036, China), Huaxue Shiji, 2017, 39(6)
Abstract: A series of benzoisoxazoles were synthesized in a one-pot process from o-nitrobenzaldehyde and sodium azide in N-methyl pyrrolidone (NMP) with inexpensive CuSO4.5H2O and sodium ascorbate as the catalyst. The process has considerable advantages in terms of the use of easily available substrates, the product diversity, the high yiled and the mild reaction conditions. The structure of the target compounds was confirmed by 1HNMR, 13CNMR, MS and element analysis.
Key words: CuSO4.5H2O; benzoisoxazoles; one-pot; synthesis
1-(2-羟基-3-甲氧苯基)乙酮的合成
杨芳芳a，张梦辉a，黄筑艳b，赵春深*b, c
(贵州大学 a. 化学与化工学院，b. 药学院，c. 贵州省发酵工程与生物制药重点实验室，贵州 贵阳 550003)
摘要：1-(2-羟基-3-甲氧苯基)乙酮是一个重要的有机中间体。以邻香兰素为起始原料，经苄基保护、烃化、氧化、脱保护4步反应合成了标题化合物。该方法具有原料廉价易得、操作简便易控、反应条件温和的优点，总收率为66.3%。
关键词：邻香兰素；1-(2-羟基-3-甲氧苯基)乙酮；合成方法
中图分类号：O625.4 文献标识码：A 文章编号： 0258-3283（2017）
Synthesis of 1-(2-Hydroxy-3-methoxyphenyl)-ethanone YANG Fang-fanga, ZHANG Meng-huia, HUANG Zhu-yanb, ZHAO Chun-shen *b, c (a. School of Chemistry and Chemical Engineering, b. School of Pharmacy, c. Key Laboratory of Guizhou for Fermentation Engineering and Biomedicine, Guizhou University, Guiyang 550003, China）, Huaxue Shiji, 2017, 39(6)
Abstract: In this work, 3-methoxysalicylaldehyde as a starting material, after the benzyl protecting, alkylation, oxidation, de-benzyl four step reaction, the title compound was synthesized. And the synthesis of the starting raw materials, low cost, easy to operate and easy to control, mild reaction conditions, the total yield of 66.3%.
Key words：3-methoxysalicylaldehyde; 1-(2-hydroxy-3-methoxy-phenyl)-ethanone; synthesis
