几种杂原子元素在天然药物分子库中的形式和意义
高文超1,2，姜雪峰*2
(1.太原理工大学 生物医学工程学院，山西 太原 030024；
2.华东师范大学 化学与分子工程学院 上海市绿色化学与化工过程绿色化重点实验室，上海 200062)
摘要：天然药物分子是药物分子库的重要组成部分，其药理活性不但与分子中的药效基团及骨架结构密切相关，而且与分子的元素组成也有重要联系。除了碳（C）、氢（H）、氧（O）、氮（N）这4种核心元素外，几种杂原子元素（S、P、Cl、Br、I）在天然药物分子也频繁出现，并对药物发挥药效起到关键作用。列举了天然药物分子中出现频率较高的上述几种杂原子元素以及含有这些元素的药物分子，并对其来源、结构、作用以及临床价值进行了简要介绍。
关键词：杂原子元素；天然药物；元素化学；药理活性；药物分子库
中图分类号：O629, 文献标识码：A 文章编号：0258-3283（2020）
Brief Analysis of the Form and Significance of Medicinal Natural Products Containing Heteroatom Elements GAO Wen-chao1,2, JIANG Xue-feng*2 (1.College of Biomedical Engineering, Taiyuan University of Technology, Taiyuan 030024, China; 2.Shanghai Key Laboratory of Green Chemistry and Chemical Process, School of Chemistry and Molecular Engineering, East China Normal University, Shanghai 200062, China), Huaxue Shiji, 2020, 42(1) ～
Abstract: Medicinal natural products belong to one important part of pharmaceutical library, and their pharmacological activities not only have the relationship with the pharmacophore and framework of molecules, but also contact with the component elements closely. Besides the essential elements such as carbon (C), hydrogen (H), oxygen (O) and nitrogen (N), several kinds of heteroatom elements (S, P, Cl, Br, and I) also play an important role in drugs based on natural products. This article listed the above “nonessential” heteroatoms with high-frequency occurring and medicinal natural products with these heteroatoms, containing the sources, significances and medicinal values of them were also discussed briefly.
Key word: heteroatom elements; medicinal natural products; element chemistry; pharmacological activities; pharmaceutical library
引用本文: 高文超，姜雪峰. 几种杂原子元素在天然药物分子库中的形式和意义. 化学试剂, 2020, 42(1): 1-7.
以泡沫镍为基底的纳米片层状Ni2+-Fe3+-V3+ LDHs的制备
及其电催化析氧性能研究
韩银凤*，张瑞林，李伟
（宝鸡文理学院 化学化工学院，陕西 宝鸡 721013）
摘要：电催化分解水是能量转化和储存的一种重要形式，析氧半反应是其速率决定步骤。本研究利用溶剂热法一步制备了以泡沫镍为基底的纳米片层状Ni-Fe-V LDHs催化材料，研究了N, N-二甲基甲酰胺用量、总金属离子浓度的变化对产物的物相、形貌、电催化析氧性能的影响，对产物进行了XRD、SEM、I/E、EIS等表征。研究结果表明，当N, N-二甲基甲酰胺用量为5 mL，总金属离子浓度为40 mmol/L时所得的Ni-Fe-V LDHs的纳米片，在1 mol/L KOH介质中，电流密度为10 mA/cm2时，其析氧超电势仅为267 mV，具有优异的电催化析氧性能。
关键词：Ni-Fe-V LDHs；纳米片；析氧半反应；N, N-二甲基甲酰胺
中图分类号：TQ630 文献标识码：A 文章编号：0258-3283（2020）
Preparation and Electrolytic Oxygen Evolution Performance Characteration of Ni2+-Fe3+-V3+ LDHs with Nanosheet Structure Based on Foam Nickel HAN Yin-feng*, ZHANG Rui-lin, LI Wei（College of Chemistry and Chemical Engineering, Baoji University of Arts and Sciences, Baoji 721013, China）, Huaxue Shiji, 2020, 42(01), ～
Abstract: Electrocatalytic water splitting is an important path of energy conversion and storage, and xygen evolution reaction (OER) is a rate-determining step in the water splitting reaction. In this study, the catalytic materials of Ni-Fe-V LDHs with nanosheet structure based on foam Nickel were prepared by solvent thermal method. It was investigated that the products on the phase, morphology and electrocatalytic oxygen evolution performance were influenced by the amount of N, N-dimethylformamide and the total metal ions concentration, and the product were characterized by XRD, SEM, I/E and EIS et al. The results showed that oxygen evolution overpotential of the obtained Ni-Fe-V LDHs with nanosheet structure when the volume of N, N-dimethylformamide is 5 mL and the total metal ion concentration is 40 mmol/L is only 267 mV in 1mol/L KOH medium and at a current density of 10 mA/cm2, which had excellent electrocatalytic oxygen evolution performance.
Key words: Ni-Fe-V LDHs; nanosheet; catalytic oxygen evolution reaction; N, N-dimethylformamide
引用本文: 韩银凤，张瑞林，李伟. 以泡沫镍为基底的纳米片层状Ni2+-Fe3+-V3+ LDHs的制备及其电催化析氧性能研究. 化学试剂, 2020, 42(1): 8-12.
C/Fe-Bi2MoO6光催化降解诺氟沙星的模拟研究
陈世界*1，张广山2，陈男1，陈茜1，黄莹莹1，吕仁江1，杨郦1
（1.齐齐哈尔大学 化学与化学工程学院，黑龙江 齐齐哈尔 161006；2.哈尔滨工业大学 环境学院，黑龙江 哈尔滨 150090）
摘要：通过水热法制备C/Fe-Bi2MoO6，样品的形貌及微观结构通过SEM、XPS、PL等手段进行表征。对光催化降解诺氟沙星(NOR)进行了研究，使用响应面方法(RSM)对光催化过程中的影响因素( pH、C/Fe-Bi2MoO6浓度、H2O2的浓度、诺氟沙星的浓度) 进行了探讨和分析，构建响应面模型，并对反应条件进行了优化。此响应面模型能够较好地模拟实验结果。优化的最佳反应条件为：pH 6.98、209.36 mg/L H2O2、1.47 g/L C/Fe-Bi2MoO6、10.54 mg/L NOR，预测和实验最大诺氟沙星去除率分别为94.54%、92.58%，数值比较接近，说明此响应面模型能够有效描述光催化反应过程，优化光催化反应条件。
关键词：C/Fe- Bi2MoO6；光催化降解；诺氟沙星；响应曲面法；模拟
中图分类号：X703 文献标识码：A 文章编号：0258-3283（2020）
A Simulating Study of C/Fe-Bi2MoO6 Photocatalytic Degradation of Norfloxacin Chen Shi-jie*1, Zhang Guang-shan2, Chen Nan1, Chen Xi1, Huang Ying-ying1, Lv Ren-jiang1, Yang Li1 (1.College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, China; 2.School of Environment, Harbin Institute of Technology, Harbin 150090, China), Huaxue Shiji, 2020, 42(01), ～
Abstract: C/Fe-Bi2MoO6 was prepared by hydrothermal method. SEM, XPS and PL were employed to characterize C/Fe-Bi2MoO6. Photocatalytic degradation of norfloxacin(NOR) by C/Fe-Bi2MoO6 was investigated in a reactor. Response surface methodology (RSM) was employed to construct RSM model and optimize three parameters (pH, H2O2 concentration, C/Fe-Bi2MoO6 concentration and NOR concentration)．The quadratic model could be used to simulate the experimental results. The optimized conditions of photocatalytic degradation of NOR were as follows: pH 6.98, initial H2O2 concentration of 209.36 mg/L, C/Fe-Bi2MoO6 concentration of 1.47 g/L and NOR concentration of 10.54 mg/L. Under these conditions, the maximal NOR removal efficiency of 94.54% and 92.58% was achieved. Also, a polynomial expression modeling the reaction was obtained. The model fitted well with the experimental data，indicating the suitability of the model and the success of response surface methodology (RSM) in optimizing the conditions of photocatalysis.
Key words: C/Fe-Bi2MoO6; photocatalytic degradation; norfloxacin; response surface methodology; simulation
引用本文: 陈世界，张广山，陈男，等. C/Fe-Bi2MoO6光催化降解诺氟沙星的模拟研究. 化学试剂, 2020, 42(1): 13-18.
TEA协助层状LZH到ZnO纳米材料控制生长机制研究
张明1, 崔节虎*1, 杜秀红2, 魏春雷1, 王香平1, 王银1, 董夏晴1
（1.郑州航空工业管理学院 郑州市环境功能材料重点实验室，河南 郑州 450015；2.河南医学高等专科学校 检验系，河南 郑州 451191）
摘要：三乙醇胺（TEA）协助下类水滑石氢氧化物碱式硝酸锌(LZH)结构到二维层状氧化锌纳米片(ZnO)转变及其性能研究相对较少。以Zn(NO3)2为锌源，借助于三乙醇胺/水体系，研究制备LZH和二维氧化锌纳米片工艺条件，影响合成层状LZH和氧化锌纳米材料的各种因素。利用X-射线粉末衍射(PXRD)、扫描电镜（SEM）、红外光谱（FT-IR）、荧光光谱（PL）等技术手段对其进行解析和表征，探讨层状碱式硝酸锌和氧化锌纳米材料之间的转变机制。结果表明：在研究范围内，温度和反应时间的改变不会影响产物的组成和结构，TEA用量直接影响到合成的目标产物。首先生成Zn(OH)2，其次转化为Zn5(OH)8(NO3)2•2H2O，过渡生成[Zn5(OH)10-x•2H2O]x+，最终自组装形成层状ZnO二维纳米材料，从而实现无需焙烧控制TEA用量制备ZnO二维纳米材料。
关键词：碱式硝酸锌；氧化锌；三乙醇胺；生长机制
中图分类号：O614 文献标识码：A 文章编号：0258-3283（2020）
Study on Control Growth Mechanism from LZH to ZnO Nanomaterials Assisted by Triethanolamine ZHANG Ming 1, CUI Jie-hu*1, DU Xiu-hong2, WEI Chun-lei, WANG Xiang-ping1, WANG Yin1, DONG Xia-qing1 (1.Key Laboratory of Environment Functional Materials, Zhengzhou University of Aeronautical, Zhengzhou 450015, China; 2.Clinical Laboratory Medicine, Henan Medical College, Zhengzhou 451191, China), Huaxue Shiji, 2020, 42(01), ～
Abstract: Study on assisted transition from hydrotalcite-like hydroxides (LHSs) to two-dimensional layered zinc oxide nanosheets (ZnO) by triethanolamine (TEA) and properties of two-dimensional zinc oxide nanosheets are relatively rare. The technological conditions for preparing layered basic zinc nitrate and two-dimensional zinc oxide nanosheets were investigated using zinc (NO3)2 as zinc source and triethanolamine/water system. The factors affecting the synthesis of layered basic zinc nitrate and zinc oxide nanosheets were also discussed. The layered basic zinc nitrate and zinc oxide nanomaterials were analyzed and characterized by X-ray powder diffraction (PXRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR), photoluminescence (PL) and other technical means, and the transformation mechanism between layered basic zinc nitrate and zinc oxide nanomaterials was explored. The results showed that the changes of the temperature and reaction time were not affect the composition and structure of the product, and the amount of TEA directly affected the target product. Firstly, Zn(OH)2 was generated. Secondly, it was transformed into Zn5(OH)8(NO3)2•2H2O, and then [Zn5(OH)10-x•2H2O]x+, finally, layered ZnO nanomaterials were formed by self-assembly, which realized that different products were prepared by controlling the amount of TEA.
Key words: hydrothermal synthesis; Zinc hydroxide nitrate; Zinc oxide; TEA; growth mechanism
引用本文: 张明, 崔节虎, 杜秀红，等. TEA协助层状LZH到ZnO纳米材料控制生长机制研究. 化学试剂, 2020, 42(1): 19-24.
色氨酸酯类盐酸盐的合成及其经皮促渗活性
王运亭1，王显赫2，郭沫汝3，乔迁*1
(1. 吉林大学 珠海学院 药学与食品科学学院，广东 珠海 519041；
2. 吉林大学 生命科学学院，吉林 长春 130012)
摘要：以对甲苯磺酰氯（PTSC）、甲醇和色氨酸为原料，采用一锅法合成他达那非重要中间体色氨酸甲酯盐酸盐，对合成工艺进行了优化，且利用该方法成功合成其他目标化合物。结构均经红外、核磁以及质谱确定。同时考察了目标产物的体外透皮促渗活性及其对应的最佳用量，结果显示，色氨酸甲酯盐酸盐无论单独使用还是和薄荷醇共同作用均对阿昔洛韦的经皮渗透吸收有明显促进作用，当色氨酸甲酯盐酸盐的用量为0.6%时，无论单独使用还是和薄荷醇共同作用效果均是最好的。
关键词：对甲苯磺酰氯；酯化反应；色氨酸酯类盐酸盐；促渗活性；工艺优化；阿昔洛韦
中图分类号：O629.71 文献标识码：A 文章编号：0258-3283(2020)--
Synthesis and Penetration Enhancing Activities of Tryptophan Ester Hydrochloride WANG Yun-ting1, WANG Xian-he2, GUO Mo-ru3, QIAO Qian*1(1.School of pharmacy food science, Zhuhai College of Jilin University, Zhuhai 519041,China; 2.College of life sciences, Jilin University, Changchun 130012, China), Huaxue Shiji, 2019, 42(01), ～
Abstract：Tryptophan methyl ester hydrochloride, an important intermediate of taladafil, was synthesized in one pot from p-toluene sulfonyl chloride (PTSC), methanol and tryptophan, and the synthesis process was optimized. Other tryptophan ester hydrochlorides also were synthesized by this method. All compounds were confirmed by IR, NMR and MS. This work also investigated the transdermal penetration enhancing activity of the target product and the optimum dosage of the target product. The result showed that the transdermal absorption of acyclovir could be promoted by tryptophan methyl ester hydrochloride alone or the combination of tryptophan methyl ester hydrochloride and menthol. The dosage of 0.6% tryptophan methyl ester hydrochloride had the best penetration effect whether it was used alone or combined with menthol.
Key words：p-toluene sulfonyl chloride; esterification; tryptophan methyl ester hydrochloride; Process optimizati- on; acyclovir; penetration enhancing activity
引用本文: 王运亭，王显赫，郭沫汝，等. 色氨酸酯类盐酸盐的合成及其经皮促渗活性. 化学试剂, 2020, 42(1): 25-29.
一种用于识别Cu2+的荧光增强型化学传感器的合成及
性能研究
杨沛然a，杨云峰*a，孟宪娇b，马文兵b
（中北大学 a.理学院，b.化学工程与技术学院，山西 太原 030051）
摘要：本论文通过对香豆素母体结构进行修饰，采取7-位引入二乙基氨基供电子基团，3-位引入酰胺基吸电子基团，成功制备了一种结构简单的荧光化学传感器：7-二乙氨基-N'-（2, 4-二硝基苯基）-2-氧代-2H-色烯-3-甲酰肼(1)，并通过1H NMR、13C NMR和ESI-HR-MS对其结构进行表征。传感器1对Cu2+显示出明显的“off-on”型荧光增强响应，荧光强度增强了21.8倍，Stokes位移为2033 cm-1，检测限为0.52 μmol/L。由Job曲线可知，传感器1和Cu2+之间的配位比为2:1，通过推测，该传感器对Cu2+的识别机理属于光诱导电子转移机理(PET)。pH测试结果表明，传感器1适宜的pH范围为7～8.5。
关键词：荧光化学传感器；香豆素；Cu2+；荧光增强
中图分类号：O622.6 文献标识码：A 文章编号：0258-3283（2020）
Synthesis and Properties of a Fluorescent Enhanced Chemosensor for the Recognition of Cu2+ YANG Pei-rana, YANG Yun-feng*a, MENG Xian-jiaob, MA Wen-bingb (a.School of Science, b.School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, China), Huaxue Shiji, 2020, 42(01) ～
Abstract: In this work, a new coumarin based fluorescent chemosensor 7-(diethylamino)-N'-(2,4-Dinitrophenyl)-
2-oxo-2H-chromene-3-carbohydrazide(1) was successfully synthesized, in which diethylamino and amide were introduced as electron-donating group and electron-withdrawing group, respectively. The chemical structure of sensor 1 was confirmed by 1H NMR, 13C NMR and ESI-HR-MS. Sensor 1 showed obvious "off-on" type fluorescence enhancement response to Cu2+ ion, fluorescence intensity increased by 21.8 times, the Stokes shift was 2033 cm-1, and the detection limit was 0.52 μmol/L. To illustrate the mechanism of sensor 1 towards binding of Cu2+ ions, a Job’s plot analysis was performed, the results of Job’s plot indicated that sensor 1 and Cu2+ ion coordinated with each other with a binding stoichiometry of 2:1. After speculation, predicting that the recognition mechanism of Cu2+ by sensor 1 belong to photoinduced electron transfer mechanism (PET). And the pH test results showed that the most suitable pH range for sensor 1 was 7～8.5.
Key words: fluorescent chemosensor; coumarin; Cu2+; fluorescence enhancement
引用本文: 杨沛然，杨云峰，孟宪娇，等. 一种用于识别Cu2+的荧光增强型化学传感器的合成及性能研究. 化学试剂, 2020, 42(1): 30-34.
铁氰化钾在有机合成中的应用
高耸松
（陕西应用物理化学研究所，陕西 西安 710061）
摘要：铁氰化钾因其特殊的氧化能力，在反应中表现出了其它氧化剂所不具备的氧化特性，在有机合成领域中起着重要的作用。它可促进多种有趣的反应，如：分子内和分子间的氧化偶联、胺类脱氢、C-H键氧化羟基化、Jacobson合成法、去羰基化、肟类化合物的脱肟反应等。这些反应被广泛应用于多种配体和具有生理活性的药物及天然产物的合成中。对铁氰化钾对近几年来铁氰化钾在有机合成领域中的发展状况、相关反应机理及良好的应用前景进行了概况性介绍。这其中也包括作者对该领域的一点贡献。
关键词：铁氰化钾；有机反应；有机合成；应用；综述
中图分类号： O621.3 文献标识码：A 文章编号：0258-3283(2020)
Application of Potassium Ferricyanide in Organic Synthesis GAO Song-song (Shaanxi Applied Physics-Chemistry Research Institute, Xi’an 710061, China), Huaxue Shiji, 2019, 42(01), ～
Abstract: Because of its special oxidation capacity, potassium ferricyanide shows the oxidative characteristics that other oxidants do not have in reactions and plays an important role in organic synthesis. Various of organic reactions which could be promoted by this reagent, for example, are the intramolecular and intermolecular coupling of phenols, oxidative hydroxylation of unsaturated C—H bonds, Jacobson synthesis, decarboxylation, dehydrogenation of amines, deoximation, et al. In addition, these reactions could be widely used in the synthesis of ligands, drugs and natural products which have physiological activities. The favourable application prospect, status of development in recent years and correlative reaction mechanism of potassium ferricyanide were summarized and discussed in the work including the contribution of the author in the field of organic synthesis for years.
Key words: potassium ferricyanide; organic reactions; organic synthesis; application; review
引用本文: 高耸松. 铁氰化钾在有机合成中的应用. 化学试剂, 2020, 42(1): 35-45.
水作为反应介质参与有机反应的研究进展
林赓a，陈星华a，姜惠婷a，穆宏文a，刘文豪b，金瑛a*
（吉林医药学院 a.药学院，b.临床学院，吉林 吉林 132000）
摘要：水作为一种优秀的绿色溶剂，具有无毒无害、价格低廉、后处理简单快捷的特质，作为有机反应介质更符合“绿色化学”的要求。以水在反应过程中的作用、使用剂量为判断依据将有水参与的有机反应分类，综述了近年来有水参与的各类有机反应。探讨了水在有机反应中的不同应用和达成纯水相反应的可能性与努力方向，如修饰催化剂、使用高温水、使用相转移催化剂等方法。比较了水相反应与有机相反应的优劣，从绿色化学的角度阐明了水相反应的优越性，简单阐述了水相反应应用于工业化的部分实例。
关键词：有机不对称反应；水相；绿色化学；催化剂修饰；高温水；有机合成；相转移催化
中图分类号：O621.3 文献标识码：A 文章编号：0258-3283（2020）
Progress of Water as Reaction Medium in Organic Reactions LIN Genga, CHEN Xing-huaa, JIANG Hui-tinga, MU Hong-wena, LIU Wen-haob, JIN Yinga* (a.School of Pharmacy, b. Clinical Medicine College, Jilin Medical University, Jinlin 132000, China), Huaxue Shiji, 2020, 42(01) ～
Abstract: As an excellent green solvent, water has the characteristics of non-toxic and harmless, low price and simple and quick treatment after experiment. As an organic reaction medium, it is more in line with the requirements of “green chemistry”. In this work, the role of water in the reaction process and the dosage used as the basis for the classification of organic reactions involving water are reviewed. The various organic reactions involving water in recent years are reviewed. The different applications of water in organic reactions and the possibility and efforts of achieving pure water phase reactions, such as modifying catalysts, using high temperature water, and using phase transfer catalysts are discussed. The advantages and disadvantages of the aqueous phase reaction and the organic phase reaction were compared. The superiority of the aqueous phase reaction is elucidated from the perspective of green chemistry, and some examples of the application of the aqueous phase reaction to industrialization are briefly described.
Key words: organic asymmetric reaction; aqueous phase; green chemistry; catalyst modification; high temperature water; organic synthesis; phase transfer catalysis
引用本文: 林赓，陈星华，姜惠婷，等. 水作为反应介质参与有机反应的研究进展. 化学试剂, 2020, 42(1): 46-52.
紫外分光光度法测定核酸含量的影响因素分析
李春1，刘建涛1,2，高运华*1，王治栋1，段学欣2
（1.中国计量科学研究院 北京 100029；2.天津大学 天津 300072）
摘要：选择寡聚核苷酸、鲑鱼精单链DNA、小牛胸腺双链DNA标准物质为样本，系统研究了溶液pH变化、苯酚、丙酮、蛋白质、多糖等对紫外分光光度法测量结果的影响情况，另外考察了核糖核酸（RNA）和脱氧核糖核酸（DNA）的相互影响情况。研究发现基于分光光度法的核酸定量分析，易受溶液 pH、苯酚、丙酮、蛋白质、多糖等的影响，另外，DNA和RNA之间也会相互干扰。因此，紫外分光光度法测定核酸含量时，特别是方法用于核酸标准物质特性量值确定时，需要样品高度纯化，pH确定的条件下才能保证测量结果的准确可靠。
关键词：紫外分光光度法；核酸；含量；影响因素；pH；有机试剂
中图分类号：O657.32 文献标志码: A 文章编号：0258-3283（2019）--
Influencing Factors of Determination of Nucleic Acid Content by Ultraviolet Spectrophotometry LI Chun1, LIU Jian-tao1, 2, GAO Yun-hua*1, WANG Zhi-dong1, DUAN Xue-xin2（1. National Institute of Metrology, Beijing 100029, China; 2. Tianjin University, Tianjin 300072, China), Huaxue Shiji, 2019, 42(01), ～
Abstract: The oligonucleotide, salmon single-stranded DNA, and calf thymus double-stranded DNA were measured by UV spectrophotometry, and the effect of solution pH change, phenol, acetone, proteins and polysaccharides on the measurement were investigated. In addition, the interaction between ribonucleic acid (RNA) and deoxyribonucleic acid (DNA) was examined. The studies had found that quantitative analysis of nucleic acids based on spectrophotometry was susceptible to solution pH, phenol, acetone, protein, polysaccharides, and so on. DNA and RNA also interfered with each other. Therefore, UV spectrophotometry for the determination of nucleic acid content required high purity of the sample, and the pH was determined to ensure accurate and reliable measurement results. Especially, this method was used to determine the characteristic value of nucleic acid reference material. It needed highly purified candidate of reference material, and the determination of pH could ensure the accuracy and reliability of the characteristic value of reference material.
Key words: ultraviolet spectrophotometry; nucleic acid; content; influencing factors; pH; organic reagent
引用本文: 李春，刘建涛，高运华，等. 紫外分光光度法测定核酸含量的影响因素分析. 化学试剂, 2020, 42(1): 53-57.
银杏双黄酮高效液相色谱定量分析方法研究
罗珂，张佳丽，雷家珩，李玲，郭丽萍*
（武汉理工大学 化学化工与生命科学学院，湖北 武汉 430070）
摘要：建立HPLC法同时测定银杏植物中阿曼托黄素、白果素、银杏黄素异构体、金松双黄酮含量。银杏叶、外种皮、白果提取液的分析采用Elite Hypersil ODS2（4.0 mm × 200 mm，5 µm），以甲醇-有机酸水溶液为流动相，梯度洗脱，体积流量0.8 mL/min，检测波长330 nm，柱温35 ℃。4种成分在各自范围内均呈良好的线性关系（r ≥ 0.9993），平均加样回收率98.3% ～ 101.0% ，RSD为1.74% ～ 2.23%。银杏叶和外种皮中均含有4种单组分双黄酮，其中白果中双黄酮总量最低，银杏叶中最高。方法准确稳定，重复性好，可用于银杏中双黄酮类成分含有量的测定。
关键词：银杏；阿曼托黄素；白果素；银杏黄素异构体；金松双黄酮；HPLC
中图分类号：O657.7 文献标志码：A 文章编号：0258-3283（2020）--
Determination of Biflavonoids in Ginkgo by HPLC LUO Ke1, ZHANG Jia-li1, LEI Jia-heng1, LI Ling1, GUO Li-ping*1 (School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, China), Huaxue Shiji, 2019, 42(01), ～
Abstract: To establish a HPLC method for the determination of amentoflavone, bilobetin，ginkgetin isomers and sciadopitysin in Ginkgo. The analysis of extracts from Ginkgo leaves, seeds and exocarps was performed on a 35℃ Elite Hypersil ODS2 (4.0 mm×200 mm, 5 µm), with the mobile phase comprising of methanol-organic acid water flowing at 0.8 mL /min in a gradient elution manner, and the detection wavelength was set at 330 nm. Four biflavonoids showed good linear relationships within their own ranges (r≥0.9993), whose average recoveries were 98.3%～101.0% with the RSDs of 1.74%～2.23%. Ginkgo leaves and exocarps both contain four biflavonoids, and the total contents of four biflavonoids is the lowest in seeds and highest in leaves. The accurate, stable and reproducible method can be used for the quality control of biflavonoids from Ginkgo.
Key words: Ginkgo; amentoflavone; bilobetin; ginkgetin isomers; sciadopitysin; HPLC
引用本文: 罗珂，张佳丽，雷家珩，等. 银杏双黄酮高效液相色谱定量分析方法研究. 化学试剂, 2020, 42(1): 58-61.
煤基活性炭甲醛吸附性能直接评价方法研究
马飞龙*，石双，韩昔，韩速，陈忠和，李拥军
（宁夏尼西活性炭有限公司，宁夏 石嘴山 753200）
摘要：针对煤基活性炭对甲醛吸附性能直接评价难题，研究一种实验室快速检测与评价方法，并设计配套检测系统。经过全流程评价实验和置信度分析，验证了该方法及系统的可靠性与稳定性。研究结果表明：常温下，载气流速为0.5 L/min，恒温吸附5 h，试样最佳甲醛回收率为2.6%；以甲醛吸附率为系统的置信区间，在[1.24，1.52]的置信度为0.95；方法误差为0.5%～1%；检测上下限为0.5～2.6。该方法和系统有望用于煤基活性炭甲醛吸附性能评价。
关键词：煤基活性炭；甲醛吸附；检测评价系统；快速检测；全流程评价；甲醛回收率；置信度分析
中图分类号： 文献标识码：A 文章编号：0258-3283（2020）
Direct Evaluation Method of Formaldehyde Adsorption Properties of Coal-based Activated Carbon MA Fei-long, SHI Shuang, HAN Xi, HAN Su, CHEN Zhong-he, LI Yong-jun (Ningxia Nixi Activated Carbon Co., Ltd., Shizuishan 753200, China), Huaxue Shiji, 2020, 42(01), ～
Abstract: A rapid laboratory testing and evaluation methods for direct evaluation of formaldehyde absorption performance of coal based activated carbon was investigated. Through the whole of processing evaluation experiment, the reliability and stability of the method and the system are verified. At room temperature the results showed that when the gas flow rate was 0.5 L/min, the constant temperature adsorption was 5 h, the optimum formaldehyde recovery of the sample was 2.6%. Taking formaldehyde adsorption rate as the confidence interval of the system, the confidence level was 0.95 in [1.24, 1.52] and the relative error was 0.5% to 1%, the method error was 0.5% to 1%, the upper and lower limits of detection was from 0.5 to 2.6. The method and system were expected to be used to evaluate the adsorption properties of formaldehyde based activated carbon.
Key words: coal based activated carbon; formaldehyde adsorption; testing and evaluation system; rapid detection; whole process evaluation; formaldehyde recovery; confidence analysis
引用本文: 马飞龙，石双，韩昔，等. 煤基活性炭甲醛吸附性能直接评价方法研究. 化学试剂, 2020, 42(1): 62-65.
电还原邻氯硝基苯合成2,2’-二氯氢化偶氮苯
电解液的高效液相色谱分析法
晋朋姣，殷跃，李彦威*
（ 太原理工大学 化学化工学院 山西 太原 030024）
摘要：实验建立了一种分析测定邻氯硝基苯电还原产物的高效液相色谱法。选用Shim-pack VP-BDS（250 mm×4.6 mm，5 μm）色谱柱，245 nm为检测波长，流动相70%甲醇，流速1.2 mL/min，柱温30 ℃，以外标法对邻氯硝基苯、邻氯苯胺和2,2’-二氯氢化偶氮苯进行定量分析。实验结果显示，在5.0～65.0 μg/mL范围内，色谱峰面积与其浓度都具有良好的线性关系，相关系数分别为r ＝ 0.9993(n ＝ 13)，r ＝ 0.9993(n ＝ 13)，r ＝ 0.9990(n ＝ 13)，且方法的精密度良好，相对标准偏差分别为≤1.41%、≤0.65%和≤1.04%。将方法应用于以邻氯硝基苯为原料电解合成2,2’-二氯氢化偶氮苯过程中产物、副产物与剩余原料的测定，其加标回收率分别在91.3%～109.4%、90.9%～103.0%和92.3%～109.7%之间，表明方法可以同时测定邻氯硝基苯、邻氯苯胺和2,2’-二氯氢化偶氮苯的含量。
关键词：高效液相色谱法；定量分析；2,2’-二氯氢化偶氮苯；邻氯硝基苯；邻氯苯胺
中图分类号：O657.7 文献标识码：A 文章编号：0258-3283（2020）--
High Performance Liquid Chromatography Method for the Electrolyte of Electro-reduction of o-Chloronitrobenzene to 2,2'-Dichlorohydrazobenzene JIN Peng-jiao, YIN Yue, LI Yan-wei* (Shanxi Institute of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024, China), Huaxue Shiji, 2019, 42(01), ～
Abstract: A HPLC method was established for the detection of the electroreduced o-chloronitrobenzene reaction product. The experiment was carried on a Shim-pack VP - BDS chromatographic column (250 mm×4.6 mm, 5μm), the detection wavelength was 245 nm, mobile phase was 70% methanol, the flow rate was 1.2 mL/min, and the column temperature was 30 ℃. Quantitative analysis of o-chloronitrobenzene, o-chloraniline and 2,2'-dichlorohydrogenazobenzene by external standard method. The peak area and its concentration show a good linear relationship in the range of 5.0～65.0 μg/mL, and the correlation coefficients were r ＝ 0.9993 (n ＝ 13), r ＝ 0.9993 (n ＝ 13), r ＝ 0.9990 (n ＝ 13), and the precision of this method was good with the relative standard deviations were ≤1.41%, ≤0.65% and ≤1.04%, respectively. The method was applied to the determination of products, by-products and remaining raw materials in the process of electrolytic synthesis of 2,2'-dichlorohydrogenazobenzene with o-chloronitrobenzene as raw material. The recoveries were 91.3%～109.4%, 90.9%～103.0% and 92.3%～109.7%, respectively, indicating that this method can be used for simultaneous determination of o-chloronitrobenzene, o-chloraniline and 2,2'-dichlorohydroazobenzene.
Key words: high performance liquid chromatography; quantitative analysis; 2,2'-dichlorohydrogenazobenzene; o-chloronitrobenzene; o-chloroaniline
引用本文: 晋朋姣，殷跃，李彦威. 电还原邻氯硝基苯合成2,2’-二氯氢化偶氮苯电解液的高效液相色谱分析法. 化学试剂, 2020, 42(1): 66-70.
液相色谱-串联质谱法测定进出口人参、西洋参中
蚜灭磷等6种农药
刘韬，高明，杨帆，张鑫，付瑶，王佳慧，张勋*
（长春海关技术中心，吉林 长春 130062）
摘要：建立了人参、西洋参中凝胶色谱-固相萃取-液相色谱-串联质谱法测定蚜灭磷、吡虫啉、涕灭威、甲基内吸磷、甲硫威、辛硫磷6种农药的分析方法。样品经丙酮超声提取，凝胶色谱（GPC）净化后，固相萃取（SPE）净化，在HPLC/MS/MS多反应监测（MRM）模式下进行了定性和定量分析方法。在上述检测方法条件下，所测的6种农药的最低检出限为0.01 mg/kg，回收率范围为79.2%～107.3%，线性范围为0.01～0.2 mg/kg。
关键词：固相萃取；人参；西洋参；农药；液相色谱-串联质谱法
中图分类号：O657.63 文献标识码：A 文章编号：0258-3283（2020）
Determination of 6 Pesticides in Imported and Exported Ginseng and Quinquefolium by High Performance Liquid Chromatography-Tandem Mass Spectrometry LIU Tao，GAO Ming，YANG Fan，ZHANG Xin，FU Yao，WANG Jia-hui，ZHANG Xun* (Changchun Customs Technology Center, Changchun 130062, China), Huaxue Shiji, 2020, 42(01), ～
Abstract：An analytical method has been established for the determination of six pesticides: aphid, imidacloprid, aldicarb, methyl endophosphate, methyl thiourea and phoxim in ginseng as well as quinquefolium by gel permeation chromatography-solid phase extraction-liquid chromatography-tandem mass spectrometry. The samples were extracted by acetone ultrasonic extraction, purified by gel permeation chromatography (GPC) and solid phase extraction (SPE) next. Qualitative and quantitative analysis were carried out under the HPLC/MS/MS multi reaction monitoring (MRM) mode. Under the above analysis conditions, the minimum detection limit of the six pesticides was 0.01 mg/kg, the recovery rate was 79.2%～107.3%, and the linear range was 0.01～0.2 mg/kg.
Key words: solid phase extraction; ginseng; quinquefolium; pesticides; LC-MS/MS
引用本文: 刘韬，高明，杨帆，等. 液相色谱-串联质谱法测定进出口人参、西洋参中蚜灭磷等6种农药. 化学试剂, 2020, 42(1): 71-75.
蠕动泵泵管对标准物质化学相容性的研究
齐钰，段嫚雷，夏娃，孟娇然，丁敏*
（上海市计量测试技术研究院，上海 201203）
摘要：对蠕动泵泵管与标准物质的化学相容性做了相关的实验研究，挑选Tygon、Chem-Durance、Viton 3种常用于输送化学溶液的泵管对4种性质不同的滴定溶液标准物质进行浸泡实验，通过标准物质特性值变化及泵管性状变化评价了这3类泵管对溶液的影响。实验结果证明不同性质的标准物质对各类泵管的化学相容性不同。通过实验结果，推测Tygon泵管对碱性、酸性、氧化性类标准物质的耐受性较好；Chem-Durance泵管适用于酸性类标准物质；Viton泵管抗吸附性较好，对还原性标准物质表现出优异的相容性，为挑选特性合适、经济合理的灌装用泵管提供了参考依据。
关键词：蠕动泵；泵管；标准物质；化学相容性；浸泡实验；滴定溶液
中图分类号：O652.1 文献标识码：A 文章编号：0258-3283（2020）--
Chemical Compatibility of Peristaltic Pump Tube with Reference Material QI Yu, DUAN Man-lei, XIA Wa, MENG Jiao-ran, DING Min*(Shanghai Institute of Measurement and Testing Technology, Shanghai 201203, China), Huaxue Shiji, 2019, 42(01), ～
Abstract：In this work, the chemical compatibility of peristaltic pump tubes with several kinds of reference material solutions was investigated experimentally. Tygon, Chem-Durance and Viton, 3 kinds of pump tubes commonly used for transporting chemical solutions, were immersed in 4 kinds of titration solution reference materials with different properties. The effects of these 3 types of pump tubes on the solution were evaluated by the changes of the characteristic values of standard materials and the properties of pump tubes. The experimental results showed that reference materials with different properties had different chemical compatibility to different kinds of pump tubes. According to the experimental results, it was inferred that Tygon pump tube had better tolerance to alkaline, acidic and oxidative reference materials; Chem-Durance pump tube was suitable for acidic reference materials; Viton pump tube had better anti-adsorption performance and excellent compatibility with reducing reference materials. This study provided a reference for selecting suitable and economical filling pump tubes in the future.
Key words: peristaltic pump; pump tube; chemical compatibility; reference material; soaking experiment; titration solution
引用本文: 齐钰，段嫚雷，夏娃，等. 蠕动泵泵管对标准物质化学相容性的研究. 化学试剂, 2020, 42(1): 76-79.
微波促进1,3偶极反应合成螺[吲哚啉-3,2'-吡咯]-2-酮衍生物及其晶体结构
於露a，徐琳琳b，马莹c，龚潘伟c，朱松磊*c
（徐州医科大学 a.基础医学院，b.公共卫生学院，c.药学院，江苏 徐州 221004）
摘要：利用多组分1,3偶极环加成方法，在微波照射条件下合成一系列螺环结构的目标化合物，对产物进行红外光谱、核磁共振谱、高分辨质谱表征，同时通过X射线单晶衍射分析5-溴-4'-(4-氯苯基)-1'-甲基-3'-(噻吩-2-酰基)螺[吲哚啉-3,2'-吡咯啉]-2-酮的结构。单晶衍射结果表明：该晶体属于单斜晶系，空间群P2(1)/n，晶体参数为a ＝ 1.2815(1) nm, b ＝ 1.0803(1) nm, c ＝ 1.6081(1) nm, α ＝ 90°, β ＝ 92.728(1)°, γ ＝ 90°。在分子晶体结构中，吡咯啉环为了信封式构象，与吲哚啉环通过螺碳原子相连，两个环接近垂直构型，其二面角为88.89(1)°。
关键词：螺[吲哚啉-3,2'-吡咯啉]；1,3偶极反应；微波合成；晶体结构；杂环
中图分类号：O 626 文献标识码：A 文章编号：0258-3283（2020）--
Microwave-assisted Synthesis and Crystal Structure of Spiro[indoline-3,2'-pyrrolidin]-2-one Derivative by 1,3 Dipolar Reaction YU Lua, XU Lin-linb, MA Ying c, GONG Pan-wei c, ZHU Song-lei *c (a. School of Basic Medical Sciences, b. School of Public Health, c. School of Pharmacy, Xuzhou Medical University, Xuzhou 221004, China), Huaxue Shiji, 2019, 42(01), ～
Abstract: The compounds 4, 4'-aryl-1'-methyl-3'-(thiophene-2-carbonyl) spiro[indoline-3,2'- pyrrolidin]-2-ones were synthesized by microwave-assistant one-pot three-component 1,3-dipolar cyclic addition reaction and fully confirmed by IR, 1H NMR, 13C NMR, HRMS and single X-ray diffraction. The crystal of compound 4a belonged to monoclinic, space group P-2(1)/n with a ＝ 1.2815(1) nm, b ＝ 1.0803(1) nm, c ＝ 1.6081(1) nm, α ＝ 90°, β ＝ 92.728(1)°, γ ＝ 90°. In the crystal structure, the pyrrolidin ring adopted envelope configuration, which linked with the indole ring by the spiro-carbon atom. The two planes had almost vertical conformation the dihedral angle was 88.89 (1)°.
Key words: spiro[indoline-3,2'-pyrrolidin]; 1,3-dipolar addition; microwave reaction; crystal structure; heterocycles
引用本文: 於露，徐琳琳，马莹，等. 微波促进1,3偶极反应合成螺[吲哚啉-3,2'-吡咯]-2-酮衍生物及其晶体结构. 化学试剂, 2020, 42(1): 80-85.
基于苝酰亚胺席夫碱荧光探针的制备及其对镉离子的选择性识别研究
喻淼*，曹晓五
（黄淮学院 化学与制药工程学院，河南 驻马店 463000）
摘要：利用C＝N异构机制，以苝酰亚胺为骨架设计合成了一种香草醛席夫碱荧光探针，通过红外光谱和质谱对其结构进行了表征。同时利用紫外可见光谱仪和荧光光谱仪对其性能进行了研究，研究结果表明，当使用490 nm的激发波长对该化合物进行激发时，化合物对Cd2+表现出良好的选择性，在530 nm处的荧光发射峰强度显著上升。干扰实验表明，Zn2+、Cu2+和Hg2+对Cd2+的识别存在干扰，大多数金属离子对识别过程影响不大。荧光实验数据分析结果表明两者之间形成了1:1的键合关系，键合常数lgK为5.37。该荧光探针对Cd2+的检出限为0.2 nmol/L（约22.8 ng/L），可以满足水体中镉离子的检测要求。
关键词：荧光探针；Cd2+ ；苝酰亚胺；香草醛；席夫碱
中图分类号：O652.3 文献标识码：A 文章编号：0258-3283（2020）--
Preparation of Perylenimide Schiff Base Fluorescent Probe and Its Selective Recognition of Cadmium Ion YU Miao*, CAO Xiao-wu (College of Chemical and Pharmaceutical Engineering, Huanghuai University, Zhumadian 463000, China), Huaxue Shiji, 2019, 42(01), ～
Abstract：Using the mechanism of C＝N isomerization, a vanillin Schiff base fluorescent probe based on perylene skeleton has been designed and synthesized to detect Cd2+. The properties were investigated by ultraviolet-visible spectroscopy, fluorescence spectroscopy, IR, and MS. The results showed that the compound had fluorescence emission at 530 nm with excitation at 490 nm. The fluorescence experiment results indicated that the compound had good selectivity for Cd2+. The fluorescence emission of the compound at 530 nm had remarkable increased (～2.5 fold) with the addition of Cd2+. The interference experiments had shown that most metal cations had little influence on the recognition of Cd2+ except Zn2+, Cu2+ and Hg2+. At the same time, a 1:1 stereo complex had formed between the compound and Cd2+ and the bonding constant (lgK) between them was 5.37. The detection limit of the compound for Cd2+ was 0.2 nmol/L (about 23 ng/L), which met the detection requirement of cadmium ion in water.
Key words: fluorescence probe; Cd2+; peryleneimide; vanillin; Shiff base
引用本文: 喻淼，曹晓五. 基于苝酰亚胺席夫碱荧光探针的制备及其对镉离子的选择性识别研究. 化学试剂, 2020, 42(1):86-89.
Idelalisib类似物的合成及其抗肿瘤活性研究
郭振，朱雯静，韩易秀，田玉顺，金成华*
（延边大学 药学院，吉林 延吉 133002）
摘要：为了寻找高效的潜在抗肿瘤药物，设计合成Idelalisib类似物并测定其抗肿瘤活性。以2-氟-6-硝基苯甲酸为起始原料，经缩合、还原、脱保护和胺化反应等5步反应合成目标化合物，并采用MTT法对所合成的化合物进行抗肿瘤活性的测定。所有的目标化合物结构均经氢谱和高分辨质谱进行确证。其中，（S）-2-（2-（（9H-嘌呤-6-基）氨基）-3-苯基丙酰胺基）-6-氟-N-苯基苯甲酰胺的抗肿瘤活性最强，它对4种肿瘤细胞的抗肿瘤活性均优于阳性对照药物Idelalisib，具有后续研究的价值。
关键词：抗癌；合成；抑制剂；MTT法；Idelalisib类似物
中图分类号：R914.5 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis and Antitumor Activity Evaluation of Idelalisib Analogs GUO Zhen, ZHU Wen-jing, HAN Yi-xiu, TIAN Yu-shun, JIN Cheng-hua* (College of pharmacy, Yanbian University, Yanji 133002, China), Huaxue Shiji, 2019, 42(01), ～
Abstract：Idelalisib analogues were designed and synthesized and their antitumor activity was determined in order to find potential antitumor drugs with high efficacy. The target compounds were synthesized from 2-fluoro-6-nitrobencoic acid through five steps of condenstation, reduction, deprotection and amination, and the antitumor activity of the compounds was determined by MTT assay. All structures of the target compounds were confirmed by 1H NMR and HRMS. Among them, the compound (S)-2-(2-((9H-purin-6-yl)amino) -3-phenylpropanmido)6-fluoro-N-phenylbenzamide showed the most anti-tumor activity, and its anti-tumor activity on 4 tumor cell lines（Raji, SU-DHL-10, HepG-2 and A549） was better than that of the positive control drug Idelalisib, which has good follow-up research value in the future.
Key words：anti-cancer; synthesis; inhibitor; MTT assay; Idelalisib analogs
引用本文: 郭振，朱雯静，韩易秀，等. Idelalisib类似物的合成及其抗肿瘤活性研究. 化学试剂, 2020, 42(1): 90-95.
依伐卡托中间体的合成工艺改进
梁停停，王均伟，朱启华，徐云根*
（中国药科大学 药物化学系，江苏 南京 211198）
摘要：改进了依伐卡托（Ivacaftor）中间体2，4-二叔丁基-5-硝基苯基乙基碳酸酯（1）的合成工艺。原料2，4-二叔丁基苯酚经过氯甲酸乙酯保护酚羟基、硝化得到中间体1和2，4-二叔丁基-6-硝基苯基乙基碳酸酯（4）的混合物，不经柱层析纯化直接利用石油醚重结晶，以56.1%的总收率制得高纯度的中间体1，经HPLC测定中间体1的纯度为95.3%。改进后的工艺操作简单、成本低廉、易于工业化放大，为依伐卡托中间体的合成提供了一种新的、高效的制备方法。
关键词：依伐卡托；2，4-二叔丁基-5-硝基苯基乙基碳酸酯；合成；工艺改进
中图分类号：R914. 5 文献标识码：A 文章编号：0258-3283(2020)
Process Improvement on the Synthesis of the Intermediate of Ivacaftor LIANG Ting-ting, WANG Jun-wei, ZHU Qi-hua, XU Yun-gen* (Department of Medicinal Chemistry, China Pharmaceutical University, Nanjing 211198, China), Huaxue Shiji, 2020, 42(01), ～
Abstract: The synthesis of 2, 4-di-tert-butyl-5-nitrophenyl ethyl carboxylate (1), a key intermediate of Ivacaftor was improved. A mixture of compound 1 and 2, 4-di-tert-butyl-6-nitrophenyl ethyl carbonate (4) was prepared by nitration of raw material 2, 4-ditert-butyl phenol protected by ethyl chloroformate, then the mixture was recrystallized directly with petroleum ether without purifying by column chromatography. The high purity of compound 1 was prepared with a total yield of 56.1% and the purity of compound 1 was 95.3% determined by HPLC. The improved reaction condition was easy to operating, low cost, and easy to be scaled up in industrialization, providing a new and efficient method for synthesis of key intermediate 1 of Ivacaftor.
Key words: Ivacaftor; 2, 4-di-tert-butyl-5-nitrophenyl ethyl carbonate; synthesis; process improvement
引用本文: 梁停停，王均伟，朱启华，等. 依伐卡托中间体的合成工艺改进. 化学试剂, 2020, 42(1): 96-99.
卡非多的合成工艺研究
王瑾，高中良*，时荣超
（河北工业大学 化工学院，天津 300130）
摘要：目标化合物是一种可以促进认知能力，增强记忆力的中枢神经系统用药。以苯乙腈为原料与氯乙酸乙酯发生取代反应生成3-腈基-3-苯丙酸乙酯，然后在催化剂作用下发生还原反应及自身缩合，合成4-苯基-2-吡咯烷酮。在氢化钠存在下，4-苯基-2-吡咯烷酮与溴乙酸乙酯反应，生成2-氧代-4-苯基-1-吡咯烷乙酸乙酯。然后在室温下与氨水经氨解得到目标化合物。总体反应路线较其它路线成本低、反应简单、副产物少、适合工业化生产。优化后反应的总收率为71.49%，目标化合物及中间体经1HNMR表征。
关键词：老年痴呆症；苯乙腈；烷基化；氨解；卡非多
中图分类号：O625.63 文献标识码：A 文章编号：0258-3283（2020）--
Synthesis of Carphedon WANG Jin, GAO Zhong-liang*, SHI Rong-chao (School of Chemical Engineering, Hebei University of Technology, Tianjin 300130, China), Huaxue Shiji, 2019, 42(01), ～
Abstract：Phenylpiracetam is a central nervous system drug that can promote cognitive ability and enhance memory. Ethyl 3-nitrile-3-phenylpropionate (1) was synthesized from phenylacetonitrile by substitution reaction with ethyl chloroacetate. Then, 4-phenyl-2-pyrrolidone (2) was synthesized by reduction reaction and self-condensation with catalyst. In the presence of sodium hydride, 4-phenyl-2-pyrrolidone reacts with ethyl bromoacetate to form 2-oxo-4-phenyl-1-pyrrolidine ethyl acetate (3). Then the target product carphedon was obtained by ammonia hydrolysis with ammonia water at room temperature. Compared with other routes, the overall reaction route has the advantages of low cost, simple reaction and less by-products, which is suitable for industrial production. The total yield of the optimized reaction was 71.49%. The target products and intermediates were confirmed by 1HNMR.
Key words: alzheimer's disease; phenylacetonitrile; alkylation; ammonolysis; carphedon
引用本文: 王瑾，高中良，时荣超. 卡非多的合成工艺研究. 化学试剂, 2020, 42(1): 100-104.
