六方氮化硼纳米片的制备
崔如馨，孙金煜*，李韵雨，俞津，施政安
（华东理工大学 材料科学与工程学院，上海市先进聚合物材料重点实验室，上海 200237）
摘要：六方氮化硼纳米片（h-BNNSs）因其优越的导热性能而倍受大众关注。六方氮化硼纳米片的大规模剥离和高质量制备方法一直是近年来研究的热点和难点，更是制约其走向应用的关键。基于此，综述了近十年来国内外先进的六方氮化硼纳米片的剥离技术和制备方法，同时分析比较不同方法的技术特点和不足，综合近年研究进展得到了六方氮化硼纳米片剥离和制备的清洁高效的方法，提出了大规模工业制备的可行性方案，对指导其工业化生产具有积极的实际意义。
关键词：六方氮化硼；纳米材料；导热性能；剥离；制备
中图分类号：TB321 文献标识码：A 文章编号：0258-3283（2019）--
Preparation of Hexagonal Boron Nitride Nanosheets CUI Ru-xin, SUN Jin-yu*, LI Yun-yu, YU Jin, SHI Zheng-an (East China University of Science and Technology, School of Materials Science and Engineering, Shanghai Key Laboratory of Advanced Polymeric Materials, Shanghai 200237), Huaxue Shiji, 2019, 41(12), ～
Abstract: Hexagonal boron nitride nanosheet (h-BNNSs) has attracted much attention due to excellent thermal conductivity. The large-scale exfoliation and high-quality preparation of h-BNNSs have been the popular issue causing great difficulties, and have become the key technologies that restrict its application. The methods of these issues were reviewed. Meanwhile the pros and cons of different methods were analyzed and compared. Based on the trend and development, a few efficient and environmental-friendly as well as large-scale preparation approaches have been proposed.
Key words: hexagonal boron nitride; nanometer material; thermal conductivity; exfoliation; synthesis
引用本文: 崔如馨，孙金煜，李韵雨，等. 六方氮化硼纳米片的制备. 化学试剂, 2019, 41(12): 1219-1227.
天然纤维素模板合成磁性铁酸钴及对酸性橙7的催化降解
陈李华,孙小霞,王雪萌,曹敏，杨雯素,牛萍*
（德州学院 化学化工学院， 山东 德州 253023）
摘要：采用溶胶-凝胶技术以天然纤维素-滤纸为模板合成磁性多孔的铁酸钴纳米材料，并采用场发射扫描电子显微镜（FFSEM）、X-射线衍射仪（XRD）和红外光谱（IR）对铁酸钴材料进行表征。铁酸钴基于体系中生成的硫酸根自由基对偶氮染料酸性橙7（AO7）表现出较高的降解活性。系统研究了铁酸盐的煅烧温度、溶液pH值、染料浓度以及无机氧化剂对降解率的影响。可磁性回收铁酸钴的使用，实现了催化剂的快速有效分离，避免了二次污染。
关键词：铁酸钴；磁性；天然纤维素；硫酸根自由基；酸性橙7
中图分类号：O611.3 文献标识码：A 文章编号：0258-3283（2019）--
Degradation of Acid Orange 7 by Magnetic Cobalt Ferrite Fabricated via Natural Cellulose Template CHEN Li-hua, SUN Xiao-xia, Wang Xue-meng, CAO Min, YANG Wen-su, NIU Ping*(College of Chemistry and Chemical Engineering, Dezhou University, Dezhou 253023, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: Cobalt ferrite porous magnetic nanomaterials were synthesized by sol-gel technology using natural cellulose-filter paper as template. The obtained nanomaterial was characterized by felid emission scanning electron microscope (FESEM), X-ray diffractometer (XRD) and infrared spectroscopy (IR). Cobalt ferrite showed high activity in degrading acid orange 7 (AO7) due to the sulfate radicals. The impact of calcinations temperature of cobalt ferrite, pH value of solution, the concentration of AO7 and inorganic oxidants on the degradation rate was investigated. The use of magnetic ferrite not only achieves the rapid and efficient separation of catalyst, but also avoids the secondary pollution.
Key words: cobalt ferrite; magnetism; natural cellulose; sulfate radicals; acid orange 7
引用本文: 陈李华,孙小霞,王雪萌,等. 天然纤维素模板合成磁性铁酸钴及对酸性橙7的催化降解. 化学试剂, 2019, 41(12): 1228-1232.
4-(4'-取代苯基)氨基-6,7-二甲氧基喹唑啉衍生物的合成与抗肿瘤活性研究
王悦秋1，梁大伟*1，魏雯2
(1. 雅安职业技术学院 药学与检验学院，四川 雅安 625000；2. 四川省肿瘤医院 肿瘤内科，四川 成都 610041)
摘要：4-(4'-羟基苯基)氨基-6,7-二甲氧基喹唑啉（WHI-P131）作为重要的JAK3激酶抑制剂，可用于治疗肿瘤及自身免疫性疾病。以临床药物WHI-P131为先导化合物，设计并合成了10个未见报道的标题化合物，其结构经IR、1HNMR与MS确证。采用MTT法，初步评价了10个新的衍生物对人宫颈癌细胞Hela、人肝癌细胞HepG2、人肺癌细胞A549、人乳腺癌细胞MCF-7与人结肠癌细胞HCT116的体外增殖抑制作用。结果表明，4’位羟基引入酰胺基团后对上述5种癌细胞的抑制作用优于母药WHI-P131，是一类潜在的抗肿瘤活性分子。
关键词：喹唑啉衍生物；药物设计；合成；JAK3；抑制剂；抗肿瘤活性
中图分类号：R914.5 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis and Antitumor Activities of 4-(4’-Substituted phenyl) amino- 6,7- Dimethoxyquinazoline Derivatives WANG Yue-qiu1, LIANG Da-wei*1, WEI Wen2 (1. School of Pharmacy & Medical Laboratory Science, Ya’an Polytechnic College, Ya’an, 625000, China; 2. Department of Oncology, Sichuan Cancer Hospital, Chengdu, 610041, China),
Abstract：The 4-(4’-hydroxyphenyl)amino-6,7-dimethoxyquinazoline (WHI-P131) is an important drug compound used as an inhibitor of JAK3 kinase, which can cure cancer and autoimmune diseases. Ten new 4-(4’-substituted phenyl)amino-6,7-dimethoxyquinazoline derivatives were synthesized with WHI-P131 as the lead compound. The structures were confirmed by IR, 1HNMR and MS. The MTT assay was used to evaluate the proliferation of five tumor cells in vitro against human cervical cancer cell Hela, human hepatocellular carcinoma cell line HepG2, human lung cancer cell A549, Human breast cancer cell MCF-7 and human colon cancer cell HCT116. The results showed that these targets with amide groups in 4’ position were novel and potential antitumor candidate compounds, which were significantly superior inhibitory activities to WHI-P131 on above cancer cells.
Key words：quinazoline derivatives; drug design; synthesis;JAK3; inhibitor; antitumor bioactivity
引用本文:王悦秋，梁大伟，魏雯. 4-(4'-取代苯基)氨基-6,7-二甲氧基喹唑啉衍生物的合成与抗肿瘤活性研究. 化学试剂, 2019, 41(12): 1233-1238.
含吗啉基片段的水杨醛席夫碱化合物的合成及其抗氧化活性
孙凤梅，胡正松
(淮阴师范学院 化学化工学院，江苏 淮安 223300)
摘要：以取代水杨醛和吗啉基苯胺缩合反应，合成了6个水杨醛席夫碱衍生物，其中3个是新化合物。其结构均经1HNMR、13CNMR、IR、LC-MS和元素分析确证。同时，通过X-单晶衍射分析，测定了2-{[(3-氟-4-吗啉苯基)亚氨基]甲基}苯酚的晶体结构，确证了化合物为稳定的E-式结构。初步测定了化合物对DPPH自由基的抗氧化活性，结果表明所有化合物在测试浓度0.02～0.10 g/L时都表现出一定的抗DPPH自由基活性。其中2-{[(3-氟-4-吗啉苯基)亚氨基]甲基}-6-甲氧基苯酚表现出优异的抗氧化活性，在不同浓度时对DPPH自由基的清除率都大于30%。
关键词：吗啉；水杨醛；席夫碱；合成；抗氧化活性
中图分类号：O625 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis and antioxidant activity of salicylaldehyde Schiff Base Containing Morpholine Fragments SUN Feng-mei ( School of Chemistry and Chemical Engineering, Huaiyin Normal University, Huai’an 223300, China ), Huaxue Shiji, 2019, 41(12), ～
Abstract：Six derivatives of salicylaldehyde Schiff bases were synthesized by condensation reaction of substituted salicylaldehyde with morpholine aniline. Their structures were confirmed by 1H NMR, 13C NMR, IR, LC-MS and elemental analysis. At the same time, the crystal structure of 2-{[(3-fluoro-4-morpholinophenyl) imino] methyl} phenol was determined by X-ray diffraction analysis, and confirmed that the compound adopted the more stable E configuration. The antioxidant activity of the compounds against DPPH free radicals was preliminarily determined, and the results showed that all compounds exhibited certain activity against DPPH free radical in the range of 0.02～0.10 g/L. 2-{[(3-Fluoro-4-morpholinophenyl) imino] methyl}-6-methoxyphenol exhibited excellent antioxidant activity, and the scavenging rate of DPPH radical was more than 30% at different concentrations.
Key words: morpholine; salicylaldehyde; Schiff base; synthesis; antioxidant activity
引用本文:孙凤梅，胡正松. 含吗啉基片段的水杨醛席夫碱化合物的合成及其抗氧化活性. 化学试剂, 2019, 41(12): 1239-1244.
含脲-喹啉受体分子的合成及其对醋酸根离子的特性荧光识别
董智云, 王拾梅, 赵三虎, 席福贵*
(忻州师范学院，山西 忻州 034000)
摘要：设计合成了含脲喹啉受体分子，并通过1HNMR、13CNMR、ESI-MS 和元素分析对其进行了结构表征。通过荧光光谱研究了受体分子对阴离子F–、Cl–、Br–、I–、AcO–、HSO4–、H2PO4–、ClO4–、NO3–的识别性能，结果发现，受体分子仅对AcO-具有荧光开启功效，Job曲线显示受体分子与AcO-的结合比为1 : 1，结合常数为(1.22±0.08)×104 L/mol。1HNMR滴定和DFT计算研究显示受体分子与AcO-形成了较强的氢键。
关键词：喹啉；脲；醋酸根；荧光探针；荧光增强
中图分类号：O625.6 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis Recogniton of Acetate Anion by Quinoline-Urea Based Receptor DONG Zhi-yun, WANG Shi-mei, ZHAO San-hu, XI Fu-gui*( Xinzhou Teachers University，Xinzhou 034000, China), Huaxue Shiji, 2019, 41(12), ～
Abstract：A novel quinoline-urea based receptor was synthesized and its structure was confirmed by 1HNMR, 13CNMR, ESI-MS and Elemental analysis. The anion binding performances of the receptor for anions F–、Cl–、Br–、I–、AcO–、HSO4–、H2PO4–、ClO4–、NO3– were evaluated by fluorescent spectroscopies, the results indicated that the receptor could behave as a “turn-on” fluorescenece sensor only for AcO-. Job-plot demonstrated that the receptor formed 1 : 1 complex with AcO-, and the binding constant is (1.22±0.08)×104 L/mol. 1HNMR titration and DFT calculation confirmed that the receptor displays strong hydrogen bonds with AcO-.
Key words：quinoline; urea; acetate; fluorescent probe; fluorescence enhancement
引用本文:董智云，王拾梅，赵三虎，等. 含脲-喹啉受体分子的合成及其对醋酸根离子的特性荧光识别. 化学试剂, 2019, 41(12): 1245-1249.
聚乙烯醇薄膜对潜在手印提取显现研究
炼铮*，路春清，朱蒋琪，宫林涛，刘先博
（中国人民公安大学 刑事科学技术学院，北京 100038）
摘要：制备了一种交联聚乙烯醇薄膜，用生物染色试剂尼罗红对其表面进行修饰，并利用制备的薄膜提取并显现多种客体表面遗留的潜在手印。实验结果表明，当尼罗红的浓度为0.1 mmol/L时，潜在手印的显现效果最佳。交联聚乙烯醇薄膜对于非渗透性客体上的潜在手印具有良好的提取和显现效果，不受客体背景、大小以及位置的影响，可以重复利用。该方法操作简单，成本低廉，为现场手印的提取显现提供了新的发展方向。
关键词：交联聚乙烯醇薄膜；尼罗红；手印显现
中图分类号：O635.1 文献标识码：A 文章编号：0258-3283（2019）--
Study of the Extraction and Development of Fingerprints by Polyvinyl Alcohol Films Lian Zheng*, Lu chun-qing, Zhu Jiang-qi, Gong Lin-tao, Liu Xian-bo (School of Forensic Science, People’s Public Security University of China, Beijing 10038, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: A cross-linked polyvinyl alcohol film was prepared and its surface was modified by biological stain agent Nile red. The film was used for extraction and development of latent fingerprints left on the objects. The results showed that when the concentration of Nile red is 0.1 mmol/L, the fingerprint development showed the best effect. The cross-linked polyvinyl alcohol film has a good extraction and developing effect on the potential fingermarks on impervious objects, and it is not affected by the background, size and location of objects. In addition, the films can be reused. This method is simple, low cost and easy to operate, which provides a new direction for extraction and development of fingerprint.
Key words: cross-linked polyvinyl alcohol film; Nile red; fingerprint development
引用本文: 炼铮，路春清，朱蒋琪，等. 聚乙烯醇薄膜对潜在手印提取显现研究. 化学试剂, 2019, 41(12): 1250-1253.
单原子催化剂的制备与表征
杨守宁a，万佳a，邓宝娟a，周萍a，薛雨燕a，姚明*b，杨嬅嬿*a
（a. 河南师范大学 化学化工学院，河南省绿色制造和精细化学品协同创新中心，教育部绿色介质与反应重点实验, 河南 新乡 453007；b. 嘉兴学院附属第一医院麻醉与疼痛医学中心，浙江 嘉兴，314001）
摘要：单原子催化剂的出现将催化研究的体系深入到了一个更加微观的尺度。单原子催化剂由于其超小的尺寸而具有许多独特的催化性能，逐渐成为近年来的研究热点，特别是通过将单原子负载于金属或金属氧化物、石墨烯、纳米颗粒等载体表面的方法，有效阻止了单原子的聚集，引起了广大科研工作者的广泛关注。基于近年来单原子领域的发展状况，总结了单原子催化剂在制备方法、表征等方面的研究现状，并对这一领域提出了展望。
关键词：单原子催化剂；制备；表征；应用；催化性能
中图分类号：O614 文献标识码：A 文章编码：0258-3283（2019）--
Preparation and characterization of single atom catalysts Yang Shou-ninga, Wan Jiaa, Deng Bao-juana, Zhou Pinga, Xue Yu-yana, Yao Ming*b, Yang Hua-yan*a (a. Collaborative Innovation Center of Henan Province for Green Manufacturing of Fine Chemicals, Henan Key Laboratory of Green Chemical Media and Reactions, School of Chemistry and Chemical Engineering, Henan Normal University, Xinxiang, 453007. b. Anesthesia and pain medical center, First affiliated hospital of jiaxing university, Jiaxing, 314001 ), Huaxue Shiji, 41(12), ～
Abstract: Researches on catalysts have deepen into a more microscopic scale with the fabrication of single atom catalysts (SACs). SACs has been developing vigorously in recent years for its unique catalytic properties, and has gradually become a research hotspot. The aggregation of single atom has been effectively prevented by loading SACs on the surface of metal or metal oxides, graphene, nanoparticles and other carriers, which has attracted widespread attention. The research status of preparation methods and characterization of single atom catalysts was summarized, and the prospect was also put forward.
Key words：single atom catalysts; preparation; characterization; application; catalyst property
引用本文: 杨守宁，万佳，邓宝娟，等. 单原子催化剂的制备与表征. 化学试剂, 2019, 41(12): 1254-1259.
绿原酸的提纯分析技术及策略
徐尤美，蔺蓓蓓，郑红星，陈琛*
（陕西理工大学 生物科学与工程学院 中德天然产物研究所，陕西 汉中 723000）
摘要：绿原酸具有抗菌，抗病毒，抗炎，保肝，降糖降脂，调节免疫、神经保护，降压，抗氧化等多种生物活性，临床上可用于抗菌解毒、消炎利胆。绿原酸易氧化、稳定性差，同分异构体较多且性质差异小，提取纯化难度大，导致绿原酸的提取率低，成本高，故绿原酸的高效提制是天然产物研究中一个热点之一。重点概述了绿原酸的提取方法，包括传统提取法、物理提取法、酶解法、超临界流体萃取法。绿原酸的纯化方法，包括膜分离、聚酰胺柱层析、大孔吸附树脂分离、高效液相色谱、高速逆流色谱法，并分析了各种方法的优缺点和应用效果，提出了绿原酸提取纯化的技术方案，为建立高效低廉的高纯度绿原酸提取纯化提供参考。
关键词：绿原酸；提取；纯化；生物活性；高纯度
中图分类号：TS201 文献标识码：A 文章编号：0258-3283（2019）--
Technology and Strategy for Extraction and Purification of Chlorogenic Acid XU You-mei, LIN Bei-bei, ZHENG Hong-xing, CHEN Chen* (Chinese-German joint Institute for natural product research, College of Biological Science and Engineering, Shaanxi University of Technology, Hanzhong 723000, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: The chlorogenic acid possess extensive physiological activity of antivirus, anti-inflammatory, hepatic- protective, hypoglycemic and hypolipidemic, immune regulation, neuroprotective, decreasing blood pressure, anti-oxidation and so on. It can be used for antibacterial disinfection, anti-inflammatory and choleretic in clinically. Due to the unique physical and chemical properties of chlorogenic acid (easy oxidation, poor stability, more isomers and small difference in properties), it is difficult to extract and purify, resulting in low extraction rate and high cost of chlorogenic acid. Therefore, the efficient extraction of chlorogenic acid is one of popular topics natural product. However, very few works have focused on reviewing the different techniques for extraction of chlorogenic acid. This work reviews extraction methods of chlorogenic acid, focuses on traditional extraction, the physical extraction, enzyme hydrolysis, and supercritical fluid extraction. The purification method of chlorogenic acid including membrane separation, column chromatography on polyamide, macroporous adsorption resins, high performance liquid chromatography, and high-speed counter-current chromatography. The advantages and disadvantages of the extraction and purification techniques of chlorogenic acid were analyzed in this work. The technical scheme of extraction and purification of chlorogenic acid was proposed, which provided a reference for the establishment of high-efficiency and low-cost extraction and purification of high purity chlorogenic acid.
Key words: chlorogenic acid; extraction; purification; biological activity; high purity
引用本文: 徐尤美，蔺蓓蓓，郑红星，等. 绿原酸的提纯分析技术及策略. 化学试剂, 2019, 41(12): 1260-1270.
螺环氧化吲哚化合物抗肿瘤活性研究进展
王碧川，陈凯镔，朱宝磊，钟伟鹏，陈清，林宁*
(广西中医药大学 药学院 广西壮瑶药工程技术研究中心，广西 南宁 530001)
摘要：研究表明含有螺环氧化吲哚骨架的化合物具有多种药理活性，如抗癌、抗炎、抗菌、抗病毒、抗疟疾和抑制胆碱酯酶等，其中抗肿瘤活性在此类骨架结构中尤为突出。根据螺环氧化吲哚骨架上 2-吲哚酮 C（3）位置上的螺杂环结构的不同进行分类，介绍近年来被报道具有抗肿瘤活性的标题化合物的研究进展，并对其作为可开发的抗肿瘤新药先导化合物的研究前景予以展望。
关键词：螺环氧化吲哚；研究进展; 药理活性；抗肿瘤；作用机制
中图分类号： 文献标识码：A 文章编号：0258-3283（2019）--
Research Progress of Anticancer Activities for Spirooxindole Compuonds Wang Bi-chuan, Chen Kai-bin, Zhu Bao-lei, Zhong Wei-peng, Chen Qing, Lin Ning* (Guangxi Zhuang Yao Medicine Center of Engineering and Technology, School of Pharmacy, Guangxi University of Chinese Medicine, Nanning 530001, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: Spirooxindoles have a variety of superior pharmacological activities, such as anticancer, antiinflammatory, antibacterial, antivirus, antimalaria and anticholinesterase. The anticancer activity is the most prominent among the biological activities of such skeletons. The progress of the different species of spiro-heterocyclic ring fused at the C(3)-position of 2-indolone was reviewed. The prospect of these compounds is also discussed as lead compounds for anticancer drugs.
Key words: Spirooxindole; research progress; pharmacological activities; anticancer; mechanisms of action
引用本文: 王碧川，陈凯镔，朱宝磊，等. 螺环氧化吲哚化合物抗肿瘤活性研究进展. 化学试剂, 2019, 41(12): 1271-1281.
神经肌肉阻断活性化合物的研究进展
肖娜1, 2，邓强1, 2，苏江涛2，柯贤炳*1
(1.武汉生物工程学院 药学院，湖北 武汉 430415；
2.湖北工业大学 生物工程与食品学院，湖北 武汉 430068)
摘要：具有神经肌肉阻断活性的药物通常称为神经肌肉阻断剂，其具有骨骼肌松弛作用，可作为手术麻醉的辅助药物广泛应用于手术的气管插管。对传统药物的化学结构进行修饰以及对新型结构化合物的探索，可得到具有神经肌肉阻断活性的新型化合物。综述总结了近几年来报道的具有潜在价值的新型神经肌肉阻断活性化合物，主要按化学结构对其进行分类，并从构效关系、药理活性等方面对这些活性化合物进行概述，为后续该类药物的开发提供一定的帮助。
关键词：神经肌肉阻断剂；神经肌肉阻断活性化合物；化学结构；构效关系；药理活性
中图分类号：R914.4 文献标识码：A 文章编号：0258-3283（2019）--
Progress in Neuromuscular Blocking Activity Compounds XIAO Na1, 2, DENG Qiang1, 2, SU Jiang-tao2, KE Xian-bing*1 (1. College of Pharmacy, Wuhan Institute of Bioengineering, Wuhan 430415, China; 2. College of Bioengineering and Food, Hubei University of Technology, Wuhan 430068, China), Huaxue Shiji, 2019, 2019, 41(12), ～
Abstract：The neuromuscular blocking active compounds which have been listed as medicine are usually called neuromuscular blocking agents. They have relaxation effect of skeletal muscle and can be widely used in tracheal intubation as auxiliary drugs of surgical anesthesia. By modifying the chemical structure of traditional drugs and exploring new structural compounds, a new type of compounds with neuromuscular blocking activity can be obtained. New neuromuscular blocking active compounds with potential value reported in recent years are summarized, which are classified base on the chemical structure, and summarized in terms of structure-activity relationship, pharmacological activity, and so on. It provides some help for the follow-up development of this kind of drugs.
Key words: neuromuscular blocking agent; neuromuscular blocking activity compound; chemical structure; structure-activity relationship; pharmacological activity
引用本文: 肖娜，邓强，苏江涛，等.神经肌肉阻断活性化合物的研究进展. 化学试剂, 2019, 41(12): 1282-1288.
HS-GC-MS法测定彩泥中28种挥发性有机物
周良春*，马俊辉，张晓飞，李双琦，杨婷，杨艳梅
（成都产品质量检验研究院有限责任公司 国家包装产品质量监督检验中心
成都市产品质量监督检验院，四川 成都 610100）
摘要：建立了顶空-气相色谱-质谱法测定彩泥中28种挥发性有机物（异丁烷、甲醇、丙酮、苯、二甲苯、乙酸乙酯等28种）的分析方法。分别讨论了顶空进样的平衡时间和平衡温度的影响，将彩泥样品经剪碎至0.5 cm×0.5 cm的颗粒，于110 ℃加热30 min后，顶空进样用质谱检测器（EI源）检测、外标法定量，可获得较好的定量结果。28种挥发性有机物在0.2～10.0 μg含量范围内，线性关系良好，各物质相关系数r均大于0.9978，方法检出限范围为0.1～0.5 mg/kg，定量限范围为0.3～1.5 mg/kg；加标平均回收率在80.5 %～105.1 %之间，相对标准偏差（n＝6）在2.1 %～9.6 %之间。该方法前处理简单、快速、准确，适用于彩泥中28种挥发性有机物的快速检测。
关键词：顶空；气相色谱质谱法；彩泥；超轻粘土；苯系物；挥发性有机物
中图分类号：O657.7 文献标识码：A 文章编号：0258-3283（2019）--
28 Volatile Organic Compounds in Colour Mud Determination by Headspace Gas Chromatography-mass Spectrometry ZHOU Liang-chun*, MA Jun-hui, ZHANG Xiao-fei, LI Shuang-qi, YANG Ting, YANG Yan-mei (Chengdu Institute of Product Quality Supervision and Inspection, National Center for Packaging Material Quality Supervision and Inspection, Chengdu Institute of Product Quality Inspection and Research Co., Ltd., chengdu 610100, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: A method was established for the determination of 28 volatile organic compounds (isobutane, methanol, acetone, benzene, dimethylbenzene and ethyl acetate, etc．) in colour mud by headspace gas chromatography-mass spectrometer(HS-GC-MS). The balance time and the balance temperature of headspace injection were investigated. VOCs were conducted by mass spectrometry detector (EI source), and the contents were calculated by the external standard method. The VOCs were well quantitatively analyzed while the headspace equilibrium temperature at 110 ℃ for 30 min with the sample diameter 0.5 cm×0.5 cm. The calibration curves were linear in the range of 0.2 ～10.0 μg with the correlation coefficients of each substance more than 0.9978. The limits of detection (LODs) were 0.1 ～ 0.5 mg/kg, the limits of quantitation (LOQs) were 0.3 ～ 1.5 mg/kg. The average recovery rate ranged from 80.5 % to 105.1 %, and the relative standard deviation (n＝6) were 2.1 ～ 9.6 %. The method is suitable for the determination of 28 VOCs in colour mud rapidly and accurately.
Keywords: headspace; gas chromatography-mass spectrometry; colour mud; ultra-light clay; benzene compounds; volatile organic compounds
引用本文: 周良春，马俊辉，张晓飞，等. HS-GC-MS法测定彩泥中28种挥发性有机物. 化学试剂, 2019, 41(12): 1289-1294.
电感耦合等离子体发射光谱法测定剥锡废液和锡泥中锡含量的方法建立
闫春辉a，金珍*a，马泓冰a，刘朋a，姚志刚a，孙宏枚b
（苏州大学 a.分析测试中心，b.材料与化学化工学部，江苏 苏州 215123）
摘要：建立了电感耦合等离子体发射光谱法（ICP-AES）测定剥锡废液和锡泥中锡含量的方法。通过处理剥锡废液和锡泥时加酸的种类、加酸量、加热温度、配置标准溶液和样品稀释时需用的介质，考察了样品的前处理方法。优化了仪器方法参数，考察了分析谱线的选择，同时对试样做了干扰试验，对方法的检出限、精密度和准确度作了讨论，考察了样品的可放置时间。将该方法应用在不同浓度的剥锡废液和锡泥中锡含量的检测，操作简便、快速，取得了满意的结果。
关键词：锡；剥锡废液；锡泥；电感耦合等离子体发射光谱法；前处理
中图分类号：O657.31 文献识别码： 文章编号：0258-3283（2019）12--
Method for Determination of Sn in Tin-stripping Waste Liquid and Tin Mud by ICP-AES YAN Chun-huia, JIN Zhen*a, MA Hong-bina, LIU Penga, YAO Zhi-ganga, SUN Hong-meib ( a. Analysis and Testing Center，b. Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: The method for determination of Sn in tin-stripping waste liquid and tin mud by inductively coupled plasma atomic emission spectrometry (ICP-AES) was set up. The method of sample treatment was investigated by treatingthe acid type, the acid content, the heating temperature and the media for the preparation of standard solution and sample dilution. The instrument parameters were optimized, the selection of analytical spectral lines was investigated, interference tests were conducted on the samples, the detection limit, degree of precision and accuracy of the method were discussed, and the storage time of the sample was investigated. The experiments of applying this method to the detection of tin content in different concentration of tin-stripping waste liquid and tin mud has proved that the method is simple and rapid in operation and satisfactory results can be achieved.
Key words: tin; tin-stripping waste liquid; tin mud; ICP–OES; pretreatment
引用本文: 闫春辉，金珍，马泓冰，等. 电感耦合等离子体发射光谱法测定剥锡废液和锡泥中锡含量的方法建立. 化学试剂, 2019, 41(12): 1295-1298.
云南烟草提取物主要生物碱的对比研究
张博1，宋凌勇*2，黄世杰2，张增辉1，郑美玲1，朱远洋1
（1. 郑州轻工业学院 食品与生物工程学院，郑州 450002；
2. 广西中烟有限责任公司技术中心，南宁 530001）
摘要：为对比分析云南烟草提取物生物碱含量的差异，建立了气相色谱-质谱联用（GC-MS）方法，并采用方法测定4种常见生物碱的含量。结果表明：4种生物碱分离度较高，相关系数≥0.9991，相对标准偏差为2.89％～4.59％，检出限0.29～0.94 μg/mL。在3个加标浓度下，平均回收率90.23％～103.71％。4种生物碱，重组分中含量最高，之后依次是净油、浸膏、轻组分。综合考虑，轻组分效果最佳。
关键词：烟草浸膏；烟草净油；轻组分；重组分；气相色谱-质谱联用（GC-MS）；生物碱
中图分类号：O0657.7+1 文献标识码：A 文章编号：0258-3283（2019）--
Comparison of Main Alkaloid from Yunnan Tobacco Extracts ZHANG Bo1，SONG Ling-yong*2，HUANG Shi-jie2，ZHANG Zeng-hui1，ZHENG Mei-ling1，ZHU Yuan-yang1 (1. School of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450002; 2. Technology Center of Guangxi Tobacoo Industry Co., Ltd., Nanning 530001), Huaxue Shiji, 2019, 41(12), ～
Abstract: To compare the differences in alkaloid of tobacco extracts, tobacco absolute oils, light distilled components of tobacco oil, and heavy distilled components of tobacco oil, gas chromatography-mass spectrometry (GC/MS) method was established and the alkaloids of four common tobacco extracts were determined. The target compounds were well separated, the correlation coefficients were all greater than 0.9991, and the method was reproducible. The relative standard deviation was 2.89%～4.59%. The detection limit of the method was 0.29～0.94 μg/mL. The three standard concentrations were high, medium and low. The average recovery rate is 90.23%～103.71%. For nicotine, myosmine, 2,3'-bipyridine, cotinine, the highest content of heavy components, followed by the net oil, extract, light components. Considering lightly, the light component works best.
Key words: tobacco extract; tobacco absolute oil; light distilled components; heavy distilled components; gas chromatography-mass spectrometry; alkaloid
引用本文: 张博，宋凌勇，黄世杰，等. 云南烟草提取物主要生物碱的对比研究. 化学试剂, 2019, 41(12): 1299-1302.
罗丹明类Fe3+荧光探针的合成及光谱性能的研究
胡伟1，刘玉婕2，田茂忠*2，白云峰2，秦君2，陈泽忠2，侯静2，李尼浩2，冯锋*1, 2
（1.山西师范大学 化学与材料科学学院，山西 临汾 041000；
2.山西大同大学 化学与环境工程学院，山西 大同 037009）
摘要：设计并合成一种水溶性较好的新型罗丹明类荧光探针（（Z）-2-（（（1H-吡咯并[2,3-c]吡啶-3-基）亚甲基）氨基）-3',6'-双（二乙胺基）螺[异二氢吲哚-1,9'-氧杂蒽] -3-酮）（RN），通过核磁共振仪（1HNMR、13CNMR）、液质色谱联用仪对RN的结构进行了表征。测试结果表明：RN可以稳定识别Fe3+并产生较强的荧光信号；在体系V（水）：V（乙醇）=9:1中RN的水溶性较好；Job′ Plot实验证明RN与铁离子的配合比为1:1；Fe3+在1～20 μmol/L范围内与RN荧光强度保持良好的线性关系（R2 ＝ 0.9972）；RN对Fe3+有高的选择性,建立了一种快速检测Fe3+的新型分析方法。
关键词：Fe3+；荧光探针；罗丹明染料；灵敏度；选择性
中图分类号：O657.3 文献标识码：A 文章编号：0258-3283(2019)--
Synthesis and Spectral Properties of Rhodamine-based a Fe3+ Fluorescent Probe HU Wei1, LIU Yu-jie2, TIAN Mao-zhong*2, BAI Yun-feng2, QIN Jun2, CHEN Ze-zhong2, HOU Jing2, LI Ni-hao2, FENG Feng*1, 2 (1. School of Chemistry and Materials Science, Shanxi Normal University, Linfen, 041000, China; 2. College of Chemistry and Environmental Engineering, Shanxi Datong University, Datong 037009, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: A novel rhodamine-based fluorescent probe ((Z)-2-(((1H-pyrrolo[2,3-c]pyridin-3-yl)methylene) amino)-3', 6'-bis(diethylamino)spiro[isoindoline-1, 9'-xanthen]-3-one) with good water solubility was designed and synthesized. The structure of RN was confirmed by the 1HNMR, 13CNMR and HRMS. The results showed that Fe3+ can be recognized by RN with the increase of fluorescence intensity. RN has good water solubility in aqueous system (V (water): V (ethanol) ＝ 9:1). The complex ratio of the RN to the iron was determined to be 1:1 by the experiment of the Job' Plot. The concentration of Fe3+ has a good linear relationship with fluorescence intensity difference of the RN and Fe3+ complex in the range of 1～20 μmol/L (R2 ＝ 0.9972) and RN has high selectivity to Fe3+. In summary, a new analytical method for rapid detection of Fe3+ was established.
Key words: Fe3+; fluorescence probe; rhodamine dye; sensitivity; selectivity
引用本文: 胡伟，刘玉婕，田茂忠，等. 罗丹明类Fe3+荧光探针的合成及光谱性能的研究. 化学试剂, 2019, 41(12): 1303-1306.
配合物[Cu0.5(H2pma)]·H2O的合成、晶体结构及光催化性能
侯银玲*，季甲，韦胜艳，胡惠慧，郑迪双
（凯里学院 大健康学院，贵州 凯里 556011）
摘要：以4-(2',4'-二羧基苯基)-2-吡啶甲酸为配体，CuCl2•2H2O为金属盐，采用溶剂热法合成了标题配合物。单晶结构解析表明，标题配合物属于三斜晶系，P-1空间群，单胞参数a ＝ 0.7761(8) nm，b ＝ 0.7873(9) nm，c ＝ 1.2020(13) nm，α＝ 88.56(4)°，β＝ 82.92(3)°，γ＝ 67.940(19)°。配体中只有一个羧基去质子化参与配位，因此标题配合物形成单核零维结构。进一步采用元素分析、红外光谱（IR）、X射线粉末衍射（PXRD）及热重分析（TGA）对标题配合物进行了结构表征，并研究了其对甲基橙（MO）的催化降解性能。结果表明，标题配合物在可见光下能够催化降解MO，降解率达79.9%，是一种潜在的催化降解有机污染物的材料。
关键词：溶剂热合成法；配合物；晶体结构；催化降解；甲基橙
中图分类号： O614.24 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis, Crystal Structure and Photocatalytic Property of [Cu0.5(H2pma)]·H2O Compound HOU Yin-ling*, JI Jia, WEI Sheng-yan, HU Hui-hui, ZHENG Di-shuang (School of Life and Health Science, Kaili University, Kaili 556011, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: A Cu-compound [Cu0.5(H2pma)]•H2O was constructed via solvothermal synthesis method with 4-(2',4'-dicarboxylphenyl)picolinic acid and copper chloride dihydrate. X-Ray single crystal diffraction reveals that the title compound crystalized in triclinic system, P-1 space group, unit cell parameters are a ＝ 0.7761(8) nm, b ＝ 0.7873(9) nm, c ＝ 1.2020(13) nm, α＝ 88.56(4)°, β＝ 82.92(3)°, and γ＝ 67.940(19)°. Only one carboxyl group is deprotonated in the ligand and participates in the coordination, so the title compound forms a mononuclear zero-dimensional structure. The title compound was confirmed by elemental analysis, infrared spectroscopy, powder X-ray diffraction and thermogravimetric analysis. The catalytic degradation of methyl orange (MO) by the title compound was elucidated, and the results show that the title compound can degradate MO in visible light, and the degradation rate reaches 79.9%, suggesting it is a potential material for catalytic degradation of organic pollutants.
Key words: solvothermal synthesis; compound; crystal structure; catalytic degradation; methyl orange
引用本文: 侯银玲，季甲，韦胜艳，等. 配合物[Cu0.5(H2pma)]·H2O的合成、晶体结构及光催化性能. 化学试剂, 2019, 41(12): 1307-1312.
穿心莲内酯的波谱特征与结构确证
雷勇胜a，丁文宇a，赵丽娜a，康江鹏a，蒋庆峰b，潘毅a，陈蔚*a
（天津药物研究院有限公司 a.原料药研发中心，b.分析测试中心，天津 300193）
摘要：建立仪器分析方法确证穿心莲内酯的化学结构与晶型。通过元素分析、紫外吸收光谱（UV）、红外吸收光谱(IR)、高分辨质谱(HRMS)、核磁共振（NMR）、单晶 X-射线衍射法确证其结构；通过差热分析（TGA-DSC)、X-射线粉末衍射确定其晶型。通过实验证实穿心莲内酯的结构。该方法准确可行，可为穿心莲内酯的结构鉴定与晶型研究提供依据。
关键词：穿心莲内酯；结构确证；波谱分析；核磁共振
Spectral Characteristic Analysis and Structural Identification of Andrographolide LEI Yong-shenga, DING Wen-yua, ZHAO Li-naa, KANG Jiang-penga, JIANG Qing-fengb, PAN Yia CHEN Wei*a (Tianjin Institute of Pharmaceutical Research Co., Ltd, a. API R&D Center, b.Analysis and Testing Center, Tianjin 300193, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: To establish a method of analytical instruments to determinate the chemical structure and crystal type of Andrographolide. The elemental analysis , UV absorption spectrum (UV), infrared spectrum (IR), high resolution mass spectrometry (HRMS), nuclear magnetic resonance (NMR), X-ray diffraction was adopted to analyze the chemical structure of Andrographolide. TGA-DSC, X- ray powder diffraction was adopted to analyze crystal type. The structure of andrographolide was confirmed. The method is accurate and feasible, and can provide a basis for the structure identification and crystal research of Andrographolide.
Key words: Andrographolide; structure identification; spectral analysis; NMR
引用本文: 雷勇胜，丁文宇，赵丽娜，等. 穿心莲内酯的波谱特征与结构确证. 化学试剂, 2019, 41(12): 1313-1316.
含二茂铁基偶氮苯水杨醛席夫碱的合成与表征
肖文杰，万屏南，刘文琴，崔汉峰，林艳*
(江西中医药大学 药学院，江西 南昌 330004)
摘要：二茂铁席夫碱是一类重要的二茂铁衍生物，具有新颖的结构和特殊的性能，将二茂铁单元与具有分子开关性能的偶氮苯水杨醛有效对接，构建具有光控分子开关性能的简单模型。以碘代二茂铁为起始原料，经亲核取代、肼解反应得到氨基二茂铁，随后与具有不同取代基的偶氮苯水杨醛进行缩合反应，设计合成了5种结构新颖的含二茂铁结构单元的偶氮苯水杨醛席夫碱。目标产物的结构经1HNMR、13CNMR、红外光谱和元素分析进行确征。该合成方法具有操作简单、反应条件不苛刻、后处理简单等优点。
关键词：二茂铁；偶氮苯；水杨醛；席夫碱；合成
中图分类号：O625.64 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis and Characterization of Azobenzene Salicylaldehyde Schiff Base Containing Ferrocene XIAO Wen-jie1, WAN Ping-nan1, LIU Wen-qin, CUI Han-feng, LIN Yan* (School of Pharmacy, Jiangxi University of Traditional Chinese Medicine, Nanchang 330004, China), Huaxue Shiji, 2019, 41(12), ～
Abstract：Ferrocene Schiff bases are important ferrocene derivatives with novel structures and special properties. A simple model was constructed with photocontrolled molecular switches that was effectively docked with azobenzylsalicylaldehyde and ferrocene unit. A series of novel azobenzene salicylaldehyde schiff base containing ferrocene were designed and synthesized from condensation reaction with azobenzyl salicylaldehyde and aminoferrocene which obtained from nucleophilic substitution and hydrazine hydrolysis reaction using ferrocene iodide as a starting material. The structure of target products was confirmed by 1HNMR, 13CNMR, infrared spectrum and elemental analysis. The synthetic method has the advantages of simple operation, less stringent reaction conditions and simple post-treatment.
Key words: ferrocene; azobenzene; salicylaldehyde; schiff base; synthesis
引用本文: 肖文杰，万屏南，刘文琴，等. 含二茂铁基偶氮苯水杨醛席夫碱的合成与表征. 化学试剂, 2019, 41(12): 1317-1321.
双咪唑基乙二醇硼酸酯衍生物的合成与表征
贾群坡1，袁斌1，吕松1，朱素芳*2
（1. 广东工业大学 环境科学与工程学院，广东 广州 510006;
2. 佛山市环境监测站，广东 佛山 528000）
摘要：以双甘油硼酸酯为原料，采用催化氧化法制备了双甘油酸硼酸酯中间体,再使中间体与邻苯二胺或乙二胺或其衍生物进行酰胺化-环化反应，高效合成了5种标题化合物，并用IR、UV、1HNMR、13CNMR和元素分析仪表征了产物结构；采用正交试验法，优化了新化合物的合成反应条件；结果表明，影响合成的因素次序为：原料摩尔比>环化温度>酰化时间>环化时间；实验为工业地沟油水解副产物甘油的综合利用提供了新技术方法。
关键词：咪唑衍生物；甘油酸；硼酸酯；合成；表征
中图分类号：O626.24 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis and Characterization of Bis(imidazolyl) Borate Derivatives JIA Qun-po1, YUAN Bin1, LV Song1, ZHU Su-fang*2 (Faculty of Environmental Science and Engineering, Guangdong University of Technology, Guangzhou, 510006, China; 2. Foshan Environmental Monitoring Center station, Foshan, 528000, China), Huaxue Shiji, 2019, 41(12), ～
Abstract：Bis(glyceric acid) borate intermediates were prepared by catalytic oxidation from diglycerol borate. Five kinds of bis(imidazolyl) borate derivatives were synthesized efficiently by one-pot amidation-cyclization reaction of bis(glyceric acid) borate and o-phenylendiamine or ethylenediamine or their derivatives in xylene medium respectively. The structure was confirmed by IR, UV, 1HNMR, 13CNMR and organic elemental analyzer. The reaction conditions were optimized by orthogonal test. The order of the factors influencing the synthesis was as follows: the molar ratio of raw materials > the cycling reaction temperature > the acylation reaction time > the cycling reaction time. It provides a new technical method for the comprehensive utilization of glycerol, a by-product of the hydrolysis of industrial gutter oil.
Key words：imidazole derivatives; glyceric acid; borate; synthesis; characterization
引用本文: 贾群坡，袁斌，吕松，等. 双咪唑基乙二醇硼酸酯衍生物的合成与表征. 化学试剂, 2019, 41(12): 1322-1326.
含1-[4-二-(4-氟苯)甲基]哌嗪官能团的1,4-二取代-1,2,3-三氮唑衍生物的设计合成及抗肿瘤活性研究
文畅，丁勇，姜芯，吴坤，梁萌，李清寒*
（西南民族大学 化学与环境保护工程学院 四川 成都 610041）
摘要：为寻找活性强、毒性低的新抗肿瘤化合物，以二-(4-氟苯)甲基氯、哌嗪、3-溴丙炔和叠氮化钠为原料合成了12个新的标题化合物，收率为46%～86%。所有化合物的结构均经过质谱、元素分析及氢/碳核磁共振谱确证。在体外对目标化合物进行了抗白血病HL-60及肺癌A-549细胞的活性测试，结果表明，浓度为40 μmol/L时，化合物对白血病HL-60细胞的抑制率高达99.25%，IC50为3.17 μg/mL。对肺癌A-549细胞的抑制率高达97.64%，IC50为12.95 μg/mL。比较化合物的结构和活性，发现吸电子基团更有利于提高化合物的抗癌活性，因此1-取代苄基-4-{1-[(4-二-(4-氟苯基)甲基]哌嗪}甲基-1,2,3-三氮唑类衍生物值得进一步深入研究。
关键词：1-[4-二-(4-氟苯)甲基]哌嗪；3-溴丙炔；1,4-二取代-1,2,3-三氮唑；有机合成；抗肿瘤活性
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283（2019）--
Design, Synthesis and Antitumor Evaluation of Novel 1,4-Disubstituted-1,2,3- triazoles Bearing 1-[4-Bi-(4-fluorophenyl)methyl]-piperazine Group WEN Chang, DING Yong, JIANG Xin, WU Kun, LIANG Meng, LI Qing-han* (College of Chemistry and Environmental Protection Engineering, Southwest Minzu University, Chengdu, 610041, China), Huaxue Shiji, 2019, 41(12), ～
Abstract: To look for a new kind of antitumor compounds with high activity and low toxicity, twelve novel title compounds were prepared via three steps starting from bi-(4-fluorophenyl)- methylchloro, piperazine, 3-bromoprop-1-yne and sodium azide with good yield (46%～86%). The structures of the new compounds were confirmed by elemental analysis, MS, 1HNMR and 13CNMR. The newly compounds exhibited good to excellent inhibitory activity against Leukemia cell HL-60 (Inhibition up to 99.25%, IC50 up to 3.17 μg/mL) and Lung cancer cell A-549 (Inhibition up to 97.64%, IC50 up to 12.95 μg/mL) in 40 μmol/L. Comparing the structure and activity of compounds, the presence of the electron-withdrawing groups in the molecules is more conducive to improving the anticancer activity of compounds. Therefore, 1-substituted benzyl-4-{1- [(4-bis- (4-fluorophenyl) methyl] piperazine} methyl-1,2,3- triazole derivatives can be used as lead molecules of anti-cancer drugs for further research.
Key words：1-[4-bi-(4-fluorophenyl)methyl]-piperazine; 3-bromoprop-1-yne; 1,4-disubstituted-1,2,3-triazole; organic synthesis; antitumor activity
引用本文: 文畅，丁勇，姜芯，等. 含1-[4-二-(4-氟苯)甲基]哌嗪官能团的1,4-二取代-1,2,3-三氮唑衍生物的设计合成及抗肿瘤活性研究. 化学试剂, 2019, 41(12): 1327-1333.
N-(5-芳苄叉基饶丹宁)环丙沙星酰胺的合成及抗肿瘤活性
张会丽1，姜亚玲1，胡国强*2，黄文龙3
（1. 郑州工业应用技术学院 药学应用技术研究所, 河南 郑州 451100；
2. 河南大学 药学院, 河南 开封 475001；3. 中国药科大学 新药研究中心, 江苏 南京 210009）
摘要 探索抗菌氟喹诺酮向抗肿瘤活性转化的结构修饰策略。用酰氨基为环丙沙星(1)C-3羧基的电子等排体，5-芳苄叉基饶丹宁为其功能修饰基，合成了11个新N-(5-芳苄叉基饶丹宁)环丙沙星酰胺类目标化合物(6a～6k)，其结构经元素分析和光谱数据确证，评价其体外对SMMC-7721、Panc-1和HL60癌细胞株及VERO正常细胞株生长抑制活性。目标化合物抗肿瘤活性显著强于母体环丙沙星，且对VERO细胞表现出较低的细胞毒性作用，尤其是卤代苯基或硝基苯基或芳香杂环类化合物的IC50已达到微摩尔浓度，与对照阿霉素相当。芳苄叉基饶丹宁修饰的酰氨基替代C-3羧基有利于提高氟喹诺酮的抗肿瘤活性。
关键词：氟喹诺酮；环丙沙星酰胺；饶丹宁；a, b-不饱和酮；电子等排体；抗肿瘤活性
中图分类号：O629.3 文献识别码：A 文章编号：0258-3283（2019）--
Synthesis and Antitumor Activity of N-Arylidene-Rhodanine Ciprofloxacin Amides ZHANG Hui-li 1，JIANG Ya-ling 2，HU Guo-qiang *2, HUANG Wen-long 3（1. School of Pharmacy, Zhengzhou University of Industrial Technology, Zhengzhou 451199, China; 2. School of Pharmacy, Henan University, Kaifeng 475001, China; 3. Center of Drug Discovery, China Pharmaceutical University, Nanjing 210009, China), Huaxue Shiji, 2019, 41(12), ～
Abstract：To explore an efficiently structural modifition strategy for a transformation of antibacterial fluoroquinolones into an antitumor fluoroquinolones. Eleven novel N-arylidene rhodanine ciprofloxacin amide derivatives (6a～6k) were synthesized with an amide group as the bioisostere of the C-3 carboxylic group modified by a functionalized arylidene rhodanine scaffold from ciprofloxacin (1), respectively. The structures were confirmed by spectral data and elemental analysis, and the in vitro anti-cell proliferation activity against SMMC-7721, Panc-1, HL60 and VERO cells were evaluated. The title compounds showed more significant potency than ciprofloxacin along with lower cytotoxicity against the normal VERO cells than comparison doxorubicin, respectively. In particular, compounds bearing a halogen or nitro-phenyl or heteroaromatic ring showed comparable activity to comparison doxorubicin. An amide group modified by arylidene rhodanine scaffold as a bioisostere of the C-3 carboxylic acid group appears to an alternative route for the improvement of the antitumor activity.
Key words： fluoroquinolone；ciprofloxacin amide；rhodanine；a, b-unsaturated ketone； bioisostere；antitumor activity
引用本文: 张会丽，姜亚玲，胡国强，等. N-(5-芳苄叉基饶丹宁)环丙沙星酰胺的合成及抗肿瘤活性. 化学试剂, 2019, 41(12): 1334-1338.
苯甲酰基丙二酸酯类化合物的水解行为研究
赵飞，孟静，李豫安，朱锦桃*
(浙江理工大学 理学院，浙江 杭州 310018)
摘要：以苯甲酰基丙二酸酯类化合物为底物，在硫酸/醋酸/水体系条件下，经水解反应合成了苯乙酮类化合物和苯甲酸类化合物。考察了该结构中苯环上取代基及丙二酸酯的种类对反应的影响，发现酯基结构的改变会显著影响苯乙酮类化合物的收率和反应时间，取代基结构的改变对此也有一定的影响。当酯基为叔丁基时，苯乙酮类化合物的收率可达80%以上，反应时间约2～3 h。此外，还探讨了可能的水解反应机理。产物结构经1HNMR和IR 确证。
关键词：苯甲酰基丙二酸酯；水解；合成；苯乙酮类化合物；苯甲酸类化合物
中图分类号：O625.42 文献标识码：A 文章编号：0258-3283（2019）12--
Hydrolysis Behavior of Benzoyl Malonate Ester Compounds ZHAO Fei, MENG Jing, LI Yu-an, ZHU Jin-tao* (College of Science, Zhejiang Sci-Tech University, Hangzhou 310018, China), Huaxue Shiji, 2019, 41(12), ～
Abstract：Acetophenone derivatives and benzoic acid derivatives were prepared by hydrolysis of various benzoyl malonate esters under sulfuric acid/acetic acid/water reaction conditions. Influence of substituent on phenyl and malonate ester was investigated, indicating that the structure of malonate ester impacted the yield and reaction time remarkably, and when tert-butyl ester was employed, the corresponding acetophenone was obtained in up to 80% yield within 2～3 h. Substituent on phenyl influenced the reaction as well in some extend. Moreover, possible mechanism was discussed. The procedure features several advantages, such as broad compatibility, concise isolation workup and high yield, endowing it a potential in industrial production. The structures were confirmed by 1HNMR and IR.
Key words：benzoyl malonate ester; hydrolysis; synthesis; acetophenone compounds; benzoic acid compounds
引用本文: 赵飞，孟静，李豫安，等. 苯甲酰基丙二酸酯类化合物的水解行为研究. 化学试剂, 2019, 41(12): 1339-1342.
