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《化学试剂》2019年第6期中英文摘要

稳定同位素氘标记试剂的研究进展

徐仲杰,雷雯,罗勇*

(上海化工研究院有限公司 国家同位素工程技术研究中心上海分中心,上海  200062 )

 

摘要: 稳定同位素氘标记试剂是科研工作中必不可少的试剂。氘代溶剂可有效避免普通溶剂氢原子干扰,被大量用于核磁共振仪溶剂。氘标记内标试剂具有优良的示踪效果,广泛地应用于食品领域的农残检测、兽残检测、非法添加剂、药物残留检测等方面。此外,由于氘原子的良好的化学惰性,氘标记试剂还用于新药研发领域。稳定同位素氘标记试剂的合成方法主要有化学合成法及物理交换法。从核磁检测、食品安全、生命科学、药物研发等方面阐述国内外近几年稳定同位素氘标记试剂的研发新技术以及应用展望。

关键词: 稳定同位素;氘标记;合成;检测;应用

中图分类号: O652     文献标识码:A    文章编号:0258-32832019

 

Research Progress of Stable Isotope Deuterium Labeling Reagents XU Zhong-jie, LEI Wen, LUO Yong*(National Isotope Engineering Technology Research Center-Shanghai Sub-Center, Shanghai Research Institute of Chemical Industry CO.,LTD., Shanghai 200062, China), Huaxue Shiji, 2019, 41(6)

Abstract: Stable isotope deuterium labeling reagent is an essential reagent in our scientific research. Deuterium substituted solvents which can effectively avoid the interference of hydrogen atoms in common solvents are used in NMR solvents in large quantities. Deuterium labeled internal standard reagents are widely used in the field of agricultural residue detection, animal residue detection, illegal additives detection, drug residue detection because of its excellent tracer effects. In addition, deuterium labeled reagents are also used in the field of new drug development due to their excellent chemical inertia. The main synthetic methods of stable isotope deuterium labeled reagents are chemical synthesis and physical exchange. In this paper, the new technology and application prospect of stable isotope deuterium labeling reagents at home and abroad in recent years are described from the aspects of nuclear magnetic detection, food safety, life science and drug research and development.

Key words: stable isotope; deuterium labeling; synthesis; detection; application

 

硒催化绿色合成反应进展

俞磊

(扬州大学 化学化工学院,江苏 扬州  225002

 

摘要:由于硒催化剂具有价格低廉、对生态友好、可回收利用、催化过程清洁等优点,硒催化的绿色合成反应有着很好的工业应用前景。最近5年以来,硒催化的有机化学反应被广泛报道,着重研究了硒催化的绿色合成反应,利用该催化技术,开发了一系列绿色氧化方法,为制备很多精细化工中间体,如反式-1,2-环己二醇、2-取代环丁酮、烯酯、β-紫罗兰酮环氧化物、有机腈、醛酮等,提供了新的合成方法。此外,通过对比分析各反应之间的联系,已逐步探索出有机硒催化反应中选择性调控的一般规律,提出了相关的理论。对相关研究进行了回顾,并展望了这一领域的发展趋势。

关键词:硒;催化;有机合成;绿色化学 

中图分类号:O6         文献标识码 A          文章编号0258-32832019--

 

Progresses in Se-catalyzed Green Synthetic Reactions YU Lei ( School of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou, 225002) huaxue shiji, 2019, 41(6),

Abstract Investigations on Se-catalyzed reaction are just unfolding. For the low price and eco-friendly features of Se as well as the recyclable catalyst and clean reaction procedures, Se-catalyzed green synthetic reactions are of very good industrial application prospects. Se-catalyzed organic reactions have been widely reported in the past 5 years. Based on this, Se-Catalyzed green reactions and by using these catalysis technologies were investigated. A series of green oxidation methods to prepare many useful fine chemical intermediates, such as trans-1,2-hexadiol, 2-substituted cyclobutanones, vinyl esters, β-ionone epoxide, organonitriles, aldehydes, ketones etc were developed. Moreover, by comparison of the reported reactions, the rules of reaction selectivity controlling in organoselenium catalyzed reactions and proposed the related theories were preliminary explored. The advances were reviewed, which looks forward to the development trend in this field.

Key words Selenium; catalysis; organic synthesis; green chemistry

 

乙二醇催化氧化反应研究进展

宁宇峰,张建栋*,李兴,魏文珑,常宏宏,高文超*

(太原理工大学 生物医学工程学院,山西 太原  030024 )

 

摘要:乙二醇属于最简单的二元醇,其化学性质活泼,可发生酯化、醚化、氧化、缩合、脱水等反应。针对乙二醇在近年来行情低迷,产能过剩的状况,重点论述了以乙二醇为主要原料可进行的的氧化反应转化,包括化学氧化法、电化学氧化法和生物催化氧化法。详细分析了酶催化和静息细胞催化等生物法转化乙二醇合成乙醇醛、乙醇酸、乙二醛等的相关研究报道,指出了生物催化氧化法相较于传统化学氧化无可比拟的优点,并对以乙二醇为原料合成精细化学品进行了展望。

关键词:乙二醇;催化氧化;生物氧化

中图分类号: O622.3    文献标识码: A    文章编号: 0258-32832019

 

Research progress in catalytic oxidation of ethylene glycol NING Yu-feng, ZHANG Jian-dong*, LI Xing, WEI Wen-long, CHANG Hong-hong, GAO Wen-chao* (College of Biomedical Engineering, Taiyuan University of Technology, Taiyuan 030024, China), Huaxue Shiji, 2019, 41(6)

Abstract: Ethylene glycol is the simplest diol. Its properties are active and can be easily esterified, etherified, oxidized, condensed, dehydrated and so on. In recent years, the production of ethylene glycol has become overcapacity and the price pressure is more serious. This paper was focused on the oxidative transformation of ethylene glycol as the main raw material, including chemical oxidation, electrochemical oxidation and biocatalytic oxidation. The research reports about the synthesis of glycolaldehyde, glycolic acid and glyoxal from ethylene glycol using biological methods such as enzyme catalysis and resting cell catalysis are also analyzed and summarizedand pointed out the advantages of biocatalytic oxidation compared to traditional chemical oxidation. Finally, prospects for the synthesis of fine chemicals from ethylene glycol are presented as well.

Key words: ethylene glycol; catalytic oxidation; biological oxidation

 

氮杂环卡宾-(II)-1-甲基咪唑配合物催化苯并噁唑与对甲苯磺酸芳酯的C-H键直接芳基化反应

郑宛莹,刘青鲜,邵黎雄*

(温州大学 化学与材料工程学院,浙江 温州  325035)

 

摘要2-芳基苯并噁唑是一类非常重要的有机化合物。以氮杂环卡宾-(II)-1-甲基咪唑[NHC-Pd(II)-Im]配合物为催化剂,通过催化苯并噁唑与对甲苯磺酸芳酯的C-H键直接芳基化,高效合成了2-芳基苯并噁唑类化合物。使用0.05倍物质的量的NHC-Pd(II)-Im配合物为催化剂,3.5倍物质的量的LiOtBu为碱,以甲苯为溶剂,不同取代基的苯并噁唑和对甲苯磺酸芳酯在130 oC下反应12 h,以71% 92%的收率得到相应的C-H键直接芳基化产物。

关键词:氮杂环卡宾钯配合物;苯并噁唑;对甲苯磺酸芳酯;C-H芳基化

中图分类号:O621.3    文献标识码:A    文章编号:0258-32832019

 

N-Heterocyclic Carbene-Palladium(II)-1-methylimidazole Complex Catalyzed Direct C-H Bond Arylation of Benzoxazoles with Aryl Tosylates ZHENG Wan-ying, LIU Qing-xian, SHAO Li-xiong* (College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China), Huaxue Shiji, 2019, 41(6)

Abstract2-Aryl benzoxazoles are frequently found in some active compounds in the area of biology, materials sciences and natural products. In this work, 2-aryl benzoxazole compounds were synthesized by direct C-H bond arylation of benzoxazoles with aryl tosylates in the presence of N-heterocyclic carbene-palladium(II)-1-methylimidazole [NHC-Pd(II)-Im] complex. Using NHC-Pd(II)-Im (5 mol%) as the catalyst, LiOtBu (3.5 equiv) as the base, a series of benzoxazoles and aryl tosylates were examined in toluene at 130 oC for 12 h, giving the corresponding direct C-H bond arylation products in 71% 92% yields.

Key wordsN-heterocyclic carbene-palladium complex; benzoxazoles; aryl tosylates; C-H bond arylation

 

微通道混合器的研制及在微乳液制备中的应用

朱宝伟*,刘海燕,陈红,冯若凡

(营口理工学院 化学与材料工程系,辽宁 营口   115014

 

摘要:微通道混合技术具备混合均匀可控制、传质传热效率高等特点。采用COMSOL Multiphysics有限元分析软件,通过建立微通道简化模型,设置理想化参数模拟微通道传质特点,根据理论分析与模拟结果进行了微通道混合器设计和加工。实验选择聚甲基丙烯酸甲酯(PMMA)为基本材质,设计、加工了三维立体结构的切割重组型号的微通道混合器,并用于微乳液复配实验。微乳液复配实验结果显示微通道加工工艺可行,可用于油相水相的混合。

关键词:微通道;传质;模拟;加工;微乳液配制

中图分类号TQ423      文献标识码A      文章编号0258-32832019--

 

Development of  Microchannel Mixer and Application in Preparation of Microemulsion ZHU Bao-wei*, CHEN Hong,LIU Hai-yan, FENG Ruo-fan (Chemical and material Engineering Department, Yingkou Institute of Technology, Yingkou 115014,China) Huaxue Shiji, 2019, 41(5),

Abstract: The characteristics of micro channel mixing technology is mixing uniformity, controllable and high heat transfer efficiency.A finite element analysis software-the COMSOL Multiphysic was adopted to establish a micro-channel simplified model and idealized parameters was set to simulate the mass transfer characteristics of the micro channel. The design and processing technology of microchannel mixer were built based on the theoretical analysis and simulation results. Polymethyl methacrylate(PMMA) was selected as the basic material in the experiment. The cutting and reassembling microchannel mixer with three-dimensional structure was made and was used for microemulsion compounding experiments. The microemulsion blending results show that the microchannel processing technology is feasible and can be used for the mixing of oil phase and water phase.

Key words: microchannel; mass transfer; simulation; processing; microemulsion preparation

 

 

7-二乙氨基香豆素-3-烯丙端基化合物的合成及其荧光性质研究

卜明a,王海君*a,马玉坤b,王静a,李爽a,陈颂a,刘磊a,孙靖文a

(齐齐哈尔医学院 a.药学院,b.医药科学研究院,黑龙江 齐齐哈尔  161006

 

摘要:以4-二乙氨基水杨醛、丙二酸环亚异丙酯为原料,经Knoevenagel反应生成7-二乙氨基香豆素-3-羧酸,与氨基酸发生缩合反应后与3-溴丙烯反应,设计合成了37-二乙氨基香豆素-3-烯丙端基化合物。结构经1HNMR13CNMRMS等加以表征,并对其荧光性质进行测定。结果表明,3种烯丙端基化合物收率均超过70%,荧光发射峰波长分别为489498508 nm,其中化合物3c具有相对较较大的Stokes位移,对A549细胞进行染色,绿光激发时,细胞呈现出强烈的绿色荧光,成功实现细胞内荧光成像,具有良好的生物应用前景。

关键词7-二乙氨基香豆素-3-羧酸;3-溴丙烯;荧光;细胞成像

中图分类号:O626.2     文献标识码:A      文章编号:0258-32832019

 

Synthesis and Fluorescence Properties of 7-Diethylamino Coumarin-3-allyl End Group Compounds BU Ming1WANG Hai-jun*1MA Yu-kun2WANG Jing1LI Shuang1CHEN Song1LIU-Lei1SUN Jing-wen1 (1.College of Pharmacy, 2.Research Institute of Medicine & Pharmacy, Qiqihar Medical University, Qiqihar 161006, China), Huaxue Shiji, 2019,

AbstractThree 7-diethylamine coumarin-3-allyl terminal compounds were synthesized by condensation reaction of 4-diethylamine salicylaldehyde and cyclopropyl acrylate via Knoevenagel. The structures were confirmed by 1HNMR, 13CNMR and MS, and their fluorescence properties were measured. The results showed that the yields of all three allyl end compounds were over 70%, and the fluorescence emission peaks were 489nm, 498 nm and 508 nm, respectively. A549 cells stained by the compound 3c with a relatively large Stokes shift showed strong green fluorescence when stimulated by green light. Therefore, the compound 3c has been successfully realized the fluorescence imaging in cells, which has a good prospect of the biological application.

Key words7-diethylaminocoumarin-3-carboxylic acid; 3-bromopropene; fluorescence; cell imaging

 

 

纳米碳酸钙吸油值的研究

常迎星,王丹丹,巩艳萍,牛振宁*,郭俊凌

(山西兰花华明纳米材料股份有限公司,山西 晋城,048002)

 

摘要: 纳米碳酸钙作为一种无机填料,其吸油值大小决定了纳米碳酸钙的表面化学性质、下游加工应用性能,吸油值越小,颗粒的分散性越好,加工性能越好。采用正交试验法优选纳米碳酸钙的制备工艺,通过正交设计选取不同氢氧化钙浓度、晶型导向剂添加量、改性剂添加量及改性时间,经过碳化合成法合成纳米碳酸钙,对其吸油值进行考察,并对实验结果进行了极差分析。研究结果表明,影响纳米碳酸钙吸油值的主要因素是改性时间,其次是氢氧化钙浓度。通过正交试验得出最优的实验条件为反应起始温度为45 ℃时,氢氧化钙浓度8.5%,晶型导向剂添加量0.9%,改性剂添加量3.5%,改性时间2 h,此时所得纳米碳酸钙吸油值为26.37。在最优条件下,所合成的纳米碳酸钙颗粒粒径为50 100 nm,晶型为立方体形,边界清晰,硅酮胶应用实验挤出性27.36 g/min,流变性黏度0.62 mPa/s,触变环面积2 334 Pa/s,屈服值133.56 Pa

关键词:正交实验;纳米碳酸钙;氢氧化钙浓度; 晶型导向剂; 改性; 吸油值

中图分类号TQ115    文献标识码A     文章编号0258-32832019--

 

Oil Absorption Value of Nano- Calcium Carbonate CHANG Ying-xing, WANG Dan-dan, GONG Yan-ping, NIU Zhen-ning*, GUO Jun-ling (Shanxi Lanhua Huaming Nano-material Co. LTD, Jincheng 048002, China) huaxue shiji, 2019, 41(  ),

Abstract: As an inorganic filler and pigment, the oil absorption value of nano-calcium carbonate is determined by the surface chemical properties of nano-calcium carbonate, processability. Smaller oil absorption value, higher particle dispersion, better processability. Through orthogonal design, different calcium hydroxide concentration, crystal guide content, modifier and modified time were selected to synthesize nano-calcium carbonate by carbonization. Carbonization method was adopted to prepare nano-calcium carbonate. The oil absorption value was analyzed. And the order and contribution rate of every experiment factor was determined by range analysis. According to the result, the main factor of oil absorption value was the modified time, followed by the concentration of Ca(OH)2. Through orthogonal experiment, the optimal experimental condition was 8.5% Ca(OH)2 concentration, 0.9% crystal guide, 3.5% sodium stearate and the modified time 2 h. Reaction temperature was 45 . Under optimal conditions, the oil absorption value of nano-calcium carbonate was 26.37. Under optimal conditions, the synthesized nano-calcium carbonate particles have a particle size of 50-100nm, and the crystal type is cubic shape and the boundary is clear. Extrusion capacity was 27.36 g·min-1, viscosity was 0.62 mPa·s-1, thixotropic ring area was 2334 Pa·s-1, yield value was 133.56 Pa.

Key words: Orthogonal test; Nano-calcium carbonate; Ca(OH)2 concentration; Crystal guide; modifying; Oil absorption value

 

 

P21活化激酶-4及其抑制剂研究进展

李瑞娟1程卯生2王健*2

1.内蒙古医科大学 药学院,内蒙古 呼和浩特  0101102. 沈阳药科大学 基于靶点的药物设计与研究教育部重点实验室,辽宁 沈阳  110016

 

摘要: P21活化激酶4P21-activated kinase 4PAK4)为小G蛋白Rho家族的关键下游效应器,通过多种机制影响肿瘤细胞的侵袭转移、增殖、存活及凋亡,对肿瘤的发生发展起着重要作用。PAK4在多种肿瘤细胞中过度表达,并成为极具研究前景的药物靶点。近年来,已经陆续发现了多种类型的PAK4激酶抑制剂,主要对PAK4激酶的结构特征、在肿瘤的发生发展中PAK4的作用机制以及PAK4激酶抑制剂的研究进展等做总结和阐述。

关键词: P21活化激酶4;蛋白结构;作用机制;抑制剂;抗肿瘤药物

中图分类号R914       文献标识码A         文章编号:0258-32832019

 

Progress in PAK4 Kinase and Inhibitors LI Rui-juan1CHENG Mao-sheng2WANG Jian*2 1. College of Pharmacy, Inner Mongolia Medical University, Huhhot 010110, China; 2. Key Laboratory of Structure Based Drug Design & Discovery, Ministry of Education, Shenyang Pharmaceutical University, Shenyang 110016, China, Huaxue Shiji, 2019, 41(6)

Abstract: The P21-activated kinase 4 (PAK4) is a key downstream effector of the Rho family GTPases, affecting the invasion, metastasis, proliferation, survival and apoptosis of tumor cells through a variety of mechanisms, and playing an important role in the occurrence and development of tumor. PAK4 is also overexpressed in many types of cancer. Therefore, PAK4 is a promising drug target. In recent years, a variety of PAK4 kinase inhibitors have been reported. This review focused on the structure characteristics of PAK4 kinase, action mechanisms in tumorigenesis and PAK4 kinase inhibitors from related literatures.

Key words: P21-activated kinase 4; protein structure; action mechanisms; inhibitor; anticancer drug

 

Diels-Alder反应合成氧化吲哚螺环化合物研究进展

刘湘1,曹国锐1,2,李高宁*1

1.青岛科技大学 化工学院,山东 青岛  2660422.济宁市化工研究院,山东 济宁  272000

 

摘要:氧化吲哚螺环化合物是多种天然产物的核心骨架,具有抗疟、抗癌、避孕、抗高血压等多种生物活性和药物活性,因此受到有机化学家们的广泛关注。目前报道的氧化吲哚螺环化合物的方法主要有1,3-偶极环加成反应、多组分串联反应以及Diels-Alder反应等,其中Diels-Alder反应凭借其条件温和、选择性好等诸多优点,成为构建螺环化合物的高效方法。在手性催化和非手性催化两方面阐述了通过Diels-Alder反应合成氧化吲哚螺环化合物的研究方法,根据催化剂的不同对其进行了分类和总结,最后对氧化吲哚螺环化合物合成的发展趋势作出了展望。

关键词:Diels-Alder反应;氧化吲哚螺环化合物;不对称催化

中图分类号:O621.3     文献标识码:A     文章编号:0258-32832018--

 

Progress on the Synthesis of Spirooxindoles by Diels-Alder Reaction LIU Xiang1, CAO Guo-rui1,2, LI Gao-ning*11. College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China; 2. Jining Research Institute of Chemical Engineering, Jining 272000, ChinaHuaxue Shiji, 2019, 41(5)

Abstract: Spirooxindoles are the core skeleton of many natural products. They have many biological and pharmaceutical activities, such as anti-malaria, anti-cancer, contraception, anti-hypertension and so on. Therefore, they have attracted extensive attention of organic chemists. At present, the main methods reported for synthesis the spirooxindoles are 1,3-dipolar cycloaddition reaction, multi-component series reaction and Diels-Alder reaction. As an efficient method for the synthesis of spirooxindoles, Diels-Alder reaction has great advantages such as mild reaction conditions and high selectivity. Recent Diels-Alder reaction in the synthesis of spirooxindole was described by the type of catalyst. In addition, the development trend of spirooxindoles was prospected.

Key words: Diels-Alder reaction; spirooxindoles; asymmetric catalysis

 

NMR技术测定口服液中葡萄糖酸含量

冷霄云1, 2,史淑丹1,李怡然2,朱明慧2,山广志*2,刘晓娟*1

1.锦州医科大学 药学院,辽宁 锦州 121000

2.中国医学科学院北京协和医学院医药生物技术研究所,北京 100050

 

摘要建立核磁共振氢谱定量(1H qNMR)分析方法,对葡萄糖酸钙锌口服溶液中葡萄糖酸进行含量测定。采用核磁共振谱仪,脉冲序列为zgpr,氘代水为溶剂,恒温26.9 ℃;弛豫时间为20 s;采集时间为2 s;中心频率为4.701 ppm;采集次数为32次。选择δ 4.0  4.1处质子峰为葡萄糖酸定量峰,顺丁烯二酸δ 6.3处为内标峰,m(葡萄糖酸):m(内标顺丁烯二酸)在1.73 8.69范围内线性关系良好,相关系数R2 0.9995;精密度、稳定性、重复性试验的相对标准偏差(RSD)分别是1.87%1.41%1.83%;平均加样回收率为99.62%RSD 0.95%n 9)。建立的方法准确、简便、高效,不需要使用对照品,可用于葡萄糖酸钙锌口服溶液制剂中葡萄糖酸的绝对定量。

关键词:核磁共振氢谱定量;葡萄糖酸钙锌口服溶液;葡萄糖酸;顺丁烯二酸

中图分类号0482.532    文献标识码A        文章编号0258-32832019--

 

Quantitative Determination of Gluconic Acid in Oral Solution by NMR LENG Xiao-yun1,2, SHI Shu-dan1, LI Yi-ran2, ZHU Ming-hui2, SHAN Guang-zhi*2, LIU Xiao-juan*1(1.       ,Jinzhou Medical University, Jinzhou 121000, China2.Institute of Medicinal Biotechnology Chinese Academy of Medical Sciences, Beijing 100050, China), Huaxue Shiji, 2019, 41(6)

Abstract: A method of 1H qNMR was developed for the determination of gluconic acid in calcium and zinc gluconates oral solution. The 1HNMR spectra were collected at Bruker Avance HD 600 spectrometer. The pulse sequence was zgpr and the solvent was deuterated water. The 1H qNMR spectra was collected at 26.9 within 20s relaxation delay, 2s acquisition time, 4.701ppm transmitter frequency offset and 32 scanning times. Proton signal peak at δ 4.0 4.1 of gluconic acid and δ 6.3 of maleic acid were served as quantitative peaks. In the mass ratio range of 1.73~8.69, a good linear relationship was established with correlative coefficient (R2) of 0.9995 for gluconic acid. The relative standard deviation (RSD) of precision, stability, and repeatability tests were 1.87%, 1.41%, 1.83%, respectively. The average recovery was 99.62% with RSD of 0.95% (n=9). The results showed that the method had the advantages of accuracy, high sensitivity and good repeatability, and could be used for the quantification of gluconic acid in calcium and zinc gluconates oral solution without standard substance.

Key words: quantitative proton nuclear magnetic resonance; calcium and zinc gluconates oral solution; gluconic acid; maleic acid

 

 

同位素稀释质谱法测定土壤中氨基酸的含量

张鹏帅,侯捷,雷雯,杜晓宁*,侯静华

(上海化工研究院,上海  200062)

 

摘要:建立了同位素稀释质谱法测定土壤中缬氨酸、亮氨酸、异亮氨酸、苯丙氨酸共4种氨基酸含量的检测方法。通过在样品中加入同位素内标试剂——稳定同位素15N标记的氨基酸,经酸解、固相萃取等前处理手段对目标氨基酸进行提取、富集以及衍生化后,利用GC-MS/MS多反应监测(MRM)模式进行定量分析。结果表明,在线性范围内,4种氨基酸的线性相关系数(R2)均大于0.999,回收率为92.2%108%,方法检出限(LOD)为1.42.9 μg/kg,定量限(LOQ)为5.28.8 μg/kg。方法高效、重现性好,可用于土壤中氨基酸的定量检测。

关键词:土壤中氨基酸;同位素稀释;定量检测;GC-MS/MS

中图分类号:O657. 63    文献标识码:A     文章编号:0258-32832019

 

Determination of Amino Acids in Soil by Isotope Dilution Mass Spectrometry ZHANG Peng-shuai, HOU Jie, LEI Wen, DU Xiao-ning*, HOU Jing-hua (Shanghai Research Institute of Chemical Industry, Shanghai 200062, China), Huaxue Shiji, 2019, 41(6),

AbstractA method has been developed to determine the amino acid contents of proline, leucine, isoleucine and phenylalanine in soil by isotope dilution mass spectrometry. By adding 15N labeled amino acid to the sample, the target amino acid is extracted, enriched and derivatized by acid hydrolysis, solid phase extraction and other pretreatment methods, and then quantitatively analyzed by GC-MS/MS (MRM) mode. The results show that the linear correlation coefficient (R2) of the four amino acids is greater than 0.999 in the linear range, the recovery was 92.2% 106.7%, and the detection limit (LOD) of the method was 1.4 2.9 μg/kg, the qantification limit (LOQ) is 5.2 μg/kg to 8.8 μg/kg. The method is highly efficient and reproducible, and can be used for quantitative detection of amino acids in soil.

Key wordsamino acid in soil; IDMS; quantitative detection; GC-MS/MS

 

 

不同的萃取方式分析葫芦巴浸膏挥发性成分

董振山1,黄世杰2,黄善松2,李庆祥1,李小兰2,李志华2,胡志忠2,张峻松*1

(1.郑州轻工业学院 食品与生物工程学院,河南 郑州  4500022.广西中烟有限责任公司 技术中心, 广西 南宁  530001)

 

摘要:为了明确葫芦巴浸膏中挥发性成分组成、含量及不同萃取方式对葫芦巴浸膏挥发性成分萃取效果的影响。分别采用固相微萃取(SPME)、溶剂萃取(LLE)和同时蒸馏萃取(SDE)对葫芦巴浸膏中挥发性成分进行提取,利用GC-MS技术对挥发性成分进行分析鉴定。3种萃取方法共鉴定出160种挥发性成分,其中固相微萃取(SPME37种、溶剂萃取(LLE66种、同时蒸馏萃取(SDE113种,3种方式共有的16种,具有葫芦巴浸膏特征香味成分的葫芦巴内酯3种方式均能萃取出来,比较3种萃取方法可知:其中同时蒸馏萃取(SDE)和溶剂萃取(LLE)对葫芦巴浸膏中香味物质提取的更为全面,两种萃取方式共鉴定出151种。

关键字:葫芦巴浸膏;溶剂萃取;固相微萃取;同时蒸馏萃取;GC-MS

中图分类号:O657.7+1    文献标识码:A    文章编号:0258-32832019--

 

Analysis of Volatile Components of Fenugreek Extract via Different Extraction Methods for DONG Zhen-shan1, HUANG Shi-jie2, HUANG Shan-song2, LI Qing-xiang1, LI Xiao-lan2, LI Zhi-hua2, HU Zhi-zhong2, ZHANG Jun-song*1 (1. College of Food and Bioengineering, Zhengzhou University of Light IndustryZhengzhou 450002, China2. Technology Center, Guangxi China Tobacco Co., Ltd.Nanning 530001, China), Huaxue Shiji, 2019, 41(5),

AbstractIn order to clarify the composition and content of volatile components in the fenugreek extract, the effect of different extraction methods on the extraction of volatile components of fenugreek extract. The volatile components in the fenugreek extract were extracted by solid phase microextraction (SPME), solvent extraction (LLE) and simultaneous distillation extraction (SDE), and the volatile components were analyzed and identified by GC-MS. A total of 160 volatile components were identified by three extraction methods, including 37 solid phase microextraction (SPME), 66 solvent extraction (LLE), and 113 kinds of simultaneous distillation (SDE). The fenugreek lactone characteristic of the fenugreek extract can be extracted in three ways. Comparing the three extraction methods, it can be known that the simultaneous extraction (SDE) and solvent extraction (LLE) extract the aroma from the fenugreek extract. More comprehensive, a total of 151 species were identified by two extraction methods.

Key words: fenugreek extract; solvent extraction; solid phase microextraction; simultaneous distillation extraction; GC-MS

 

 水质污染监测用7种阴离子溶液标准物质的研制

张惠,张鹏辉,杨娜,高琴,方正*

(中国测试技术研究院,四川 成都  610021

 

摘要:使用电感耦合等离子体质谱仪、离子色谱仪等对研制的7种阴离子溶液标准物质原料的杂质进行定性和定量测定。通过杂质扣除法对原料纯度定值,并定量测定原料中7种离子间相互包含情况。采用重量-容量法对溶液标准物质准确定值。7种阴离子溶液可用于测定7种阴离子的分析方法确认与评价、成分定量分析等。为复杂微量样品中7种阴离子的测试参数提供参考标准。可以节约监测资源、提高效率。对监测环境水、饮用水和食品中重要阴离子和尽量保证样品检测的及时性具有重要意义。

关键词:阴离子;标准物质;杂质扣除法;复杂样品

中图分类号:O625. 11      文献标识码:A      文章编号:0258-32832019--

 

Preparation of 7 Kinds of Anions Reference Materials for Monitoring Water Pollutants ZHANG Hui, ZHANG Peng-hui, Yang Na, GAO Qin, FANG Zheng* (National Institute of Measurement and Testing Technology, Chengdu 610021) Huaxue Shiji, 2019, 41(5),

Abstract: The impurities in the raw materials of 7 kinds of anions solution reference material were determined qualitatively and quantitatively by inductively coupled plasma mass spectrometry, ion chromatograph, etc. The deduction impurity method was used to calculate definite values for raw materials. These ions were detected quantitatively which exist in each other as impurities. The weighting-volumetric method was used to define the characteristic value of this reference material. The 7 kinds of anions reference material can be used in the confirming and evaluation of analytic procedure, also quantitative analysis. It can be used as a reference standard for testing 7 anions parameters in complex micro-samples. It can economize on monitoring resources and improving efficiency. It plays an important role for monitoring anions which are present in environmental water, drinking water and food. It is also of great significance to ensure the timeliness of sample detection.

Key words: anions; reference material; deduction impurity method; complex sample

 

 

人参皂苷Rg3体外经皮渗透特性研究

史淑丹1,郑岩1,王硕2,富力2,孙玉琦*1

(1. 锦州医科大学 药学院,辽宁 锦州  121001

2. 大连富生天然药物开发有限公司,辽宁 大连  116600)

 

摘要:研究人参皂苷Rg3体外经皮渗透特性以及不同促渗剂的影响。测定人参皂苷Rg3与经皮渗透相关的物理参数。通过扩散池试验,采用HPLC法测定人参皂苷Rg3的累积透过量(Q),拟合Q-t曲线,考察体外经皮渗透性能;测定β-环糊精、吐温-80、油酸、氮酮、薄荷油的增渗倍数(ER),考察不同促渗剂对人参皂苷Rg3经皮渗透性质的影响。人参皂苷Rg3的表观溶解度为56.70 µg/mL,油水分配系数(logP)为2.63,熔点为312.2 ℃。人参皂苷Rg3经皮渗透为恒速过程,12 h累积透过量为14.45 μg/cm2;不同促渗剂对人参皂苷Rg3的促渗作用存在差异,薄荷油增渗倍数为2.38。人参皂苷Rg3体外释放符合零级过程,薄荷油对其促渗作用效果显著,可作为一种具有发展潜力的新型外用镇痛化合物。

关键词:人参皂苷Rg3;经皮渗透;促渗剂;累积透过量;增渗倍数

中图分类号:R944.9    文献标识码:A       文章编号:0258-32832019

 

Character study on percutaneous permeation of ginsenoside Rg3 in vitro SHI Shu-dan1, ZHENG Yan1, WANG Shuo2, FU Li2, SUN Yu-qi*1(1. College of Pharmacy, Jinzhou Medical University, Jinzhou 121001, China; 2. Dalin Fusheng Natural Medicine Development Co.Ltd., Dalian 116600, China), Huaxue Shiji, 2019, 41(6)

Abstrat: To investigate the percutaneous permeation character of ginsenoside Rg3 and the effects of different permeation enhancers in vitro. The physical properties of ginsenoside Rg3 were measured. The permeation of ginsenoside Rg3 was evaluated by transdermal permeation instrument. The cumulative permeation amount (Q) was determined by HPLC to fit Q-t curve. The enhancing rate (ER) of β-cyclodextrin, tween-80, oleic acid, azone or peppermint oil was calculated to investigate the enhanced effect of ginsenoside Rg3 by different permeation enhancers. The apparent solubility ofginsenoside Rg3 was 56.70 ug/mL, the logP was 2.63 and the melting point was 312.2 . Ginsenoside Rg3 had a constant rate in the percutaneous process. The Q of ginsenoside Rg3 in 12 h was 14.45 μg/cm2. Different permeation enhances showed different enhanced effects. The ER of peppermint oil was 2.38. Transdermal permeation of ginsenoside Rg3 fit the zero-order equation in vitro. Peppermint oil could enhance the permeation amount of ginsenoside Rg3 significantly.Thus, ginsenoside Rg3 is a potential new potent topical analgesic.

Key words ginsenoside Rg3; percutaneous permeation; permeation enhancer; cumulative permeation amount; enhancing rate

 

 

五爪金龙吸附阳离子染料的性能研究

杨新周a,b,杨子仙a,田先娇b,c,马艳粉b,c

(德宏师范高等专科学校 a. 理工系,b.民族医药研究所,c. 生命科学系,云南 德宏  678400)

 

摘要:以五爪金龙为原料,经粉碎制成不同粒径的粉末吸附剂,探究了五爪金龙吸附亚甲基蓝、罗丹明B、碱性品红的性能。研究发现,五爪金龙吸附亚甲基蓝、罗丹明B、碱性品红最佳粒径为0.3 mm、最佳投加量分别为1.62.60.8 gpH均为5、温度为30 ℃、震荡时间均为40 min。利用准一级、准二级动力学方程模拟五爪金龙吸附亚甲基蓝、罗丹明B和碱性品红的动力学过程,结果表明五爪金龙吸附亚甲基蓝、罗丹明B和碱性品红的过程适合于准二级动力学模型。研究热力学参数发现,五爪金龙吸附亚甲基蓝、碱性品红的过程是一个自发的趋于无序的放热过程,吸附罗丹明B的过程是一个自发的趋于有序的放热过程。

关键词:五爪金龙;亚甲基蓝;碱性品红;罗丹明B;吸附

中图分类号:X703    文献标识码:A    文章编号:0258-32832019

 

Adsorptive Performance of Ipomoea Cairica on CatioIlic Dye in Aqueous Solution

YANG Xin-zhoua,b, YANG Zi-xiana,b, TIAN Xian-jiaob,c, MA Yan-fena,c (a. Science and Engineering Department , b.The Research Institute of Ethnic Minority Medicine, c. Department of life sciences, Dehong Teachers college, Dehong 678400, China), Huaxue Shiji, 2019

Abstract:The powder of Ipomoea cairica at different particle sizes was prepared as adsorbent by crush. The adsorption properties of Ipomoea cairica powder for methylene blue, rhodamine B and basic fuchsine were investigated at various conditions. It showed that the optimal adsorption conditions were as follow: the dosage of Ipomoea cairica powder were 1.62.60.8 g, pH value were 5, particle size were 0.3 mm, adsorption time at 40 min and temperature at 30 . The pseudo-first-order, pseudo-second-order were used to simulate the kinetic process of it. The results showed that the pseudo-second kinetic equation is more suitable for describing the process of it. The thermodynamic parameters were calculated and results were as follow: in the process of Ipomoea cairica powder adsorption of methylene blue and basic fuchsine, which indicate that it is a spontaneous, disorderly and endothermic process. In the process of Ipomoea cairica powder adsorption of rhodamine B, which indicate that it is a spontaneous, orderly and endothermic process.

Key words: Ipomoea cairica, methylene blue, basic fuchsine, rhodamine B, adsorption

 

 

杂多酸离子液体催化下的过氧乙酸绿色合成工艺研究

胡珂1,康丽峰2,余定华*2

(1.  南京市第一中学,江苏 南京  2100012. 南京工业大学 药学院,江苏 南京  210009

 

摘要: 以溴化1-丁基-3-甲基咪唑([Bmim]Br)和磷钨酸(H3PW12O40)为原料制备了杂多酸型离子液体催化剂1-丁基-3-甲基咪唑磷钨酸盐([ Bmim]3PW12O40),经傅里叶变换红外光谱确证其结构,考察了催化剂对双氧水氧化冰醋酸合成过氧乙酸反应的催化活性及其催化工艺条件。实验结果表明,该杂多酸离子液体是一种新型、高效且环境友好的固相催化剂,在:V(双氧水)∶V(冰醋酸)=1.751、温度 60 ℃、催化剂用量为原料总质量的0.5%、时间4 h的优化反应条件下,过氧乙酸的浓度可达到20.3%。而且,催化剂循环使用8次后,依然保持了优异的稳定性。制备的过氧乙酸产品因不含硫酸催化剂,解决了现有浓硫酸催化方法存在的环境不友好、储存和运输存在安全隐患、产品应用领域受限等问题。

关键词:离子液体;磷钨酸;杂多酸;过氧乙酸;绿色合成

中图分类号:TQ111    文献标识码:A       文章编号:0258-32832019

 

Study on the Green Synthesis of Peracetic Acid Catalyzed by Heteropoly Acid Ionic Liquid HU Ke1, KANG Li-feng2, YU Ding-hua*2 (1. Nanjing No.1 Middle School, Nanjing 210001, China; 2. College of Pharmaceutical Science, Nanjing Tech University, Nanjing 210009, China), Huaxue Shiji, 2019, 41(6)

Abstract: Heteropolyacid ionic liquid catalyst 1-butyl-3-methyl imidazolium dodecatungstophosphate (Bmim]3PW12O40) was prepared using 1-butyl-3-methyl imidazolium bromide ([Bmim]Br) and dodecatungstophosphoric acid (H3PW12O40) as the starting materials, and which was characterized by Fourier transform infrared spectroscopy. The catalytic activity of the catalyst and its catalytic process conditions for the synthesis of peroxyacetic acid from hydrogen peroxide and glacial acetic acid was investigated. The experimental results show that the heteropolyacid ionic liquid is a novel, efficient and environmentally friendly solid phase catalyst. Under the optimized reaction conditions: volume ratio of hydrogen peroxide to glacial acid is 1.75, reaction temperature is 60 , mass ratio of catalyst to the stock solution is 0.005, the concentration of acetic acid peroxide could reach 20.3% after reaction for 4 h. Moreover, the catalyst could still maintain excellent stability after 8 times of recycling. Due to the absence of sulfuric acid catalyst, the peracetic acid products prepared by this process has solved the problems of unfriendly environment, potential safety hazards in storage and transportation, and limited application fields of products existing in the traditional concentrated sulfuric acid catalytic method.

Key words: ionic liquids; dodecatungstophosphoric acid; heteropolyacid; peroxyacetic acid; green synthesis

 

 

7-氮杂吲哚及其衍生物5--7-氮杂吲哚的合成

郑从燊1,陈夏琴1,余辉1,黄捷*1,杨帆2,汤杰2

(1. 福建省微生物研究所,福建 福州  350007; 2. 华东师范大学 化学与分子工程学院,上海  200241)

                                                                                                                                                 

摘要7-氮杂吲哚是一种重要的杂环化合物,是合成维罗非尼、ABT-199等抗肿瘤药物的重要中间体,具有较高的生物医药价值。优化了合成7-氮杂吲哚的方法,以廉价易得的2-氨基-3-甲基吡啶为起始原料,经过两步反应,以48%的总收率得到7-氮杂吲哚。并在此合成方法的基础上进一步合成了5--7-氮杂吲哚,经过三步反应,总收率达到43%。该合成方法具有原料易得、操作简便、路线简短、收率较高等优点。产物的结构经过核磁共振和高分辨质谱得到确认。

关键词:7-氮杂吲哚;5--7-氮杂吲哚;杂环;合成

中图分类号: O626.32               文献标识码:A             文章编号:0258-32832019

 

Synthesis of 7-Azaindole and 5-Bromo-7-azaindole  ZHENG Cong-shen1, CHEN Xia-qin1, YU Hui1, HUANG Jie*1, YANG Fan2, Tang Jie2(1.Fujian Institute of Microbiology, Fuzhou 350007, China; 2. School of Chemistry and Molecular Engineering, East China Normal University, Shanghai 200241, China), Huaxue Shiji, 2019, 41(6)

Abstract: 7-Azaindole compounds are important heterocyclic compounds, used for the synthesis of vemurafenib and ABT-199. New methods for the synthesis of 7-azaindole is reported herein. 7-Azaindole is synthesized from 2-amino-3-methylpyridine via a two-step synthetic route in an overall yield of 48%. 5-Bromo-7-azaindole is synthesized from 2-amino-3-methylpyridine via a three-step synthetic route in an overall yield of 43%. The product is characterized by NMR and HRMS. The advantages of this procedure include short reaction steps and good yields.

Key words: 7-azaindole; 5-bromo-7-azaindole; heterocyclic; synthesis

 

 

C22-脂环族三羧酸()的合成工艺改进

廖德仲1,占达东2,孙宏元2,赵玉玲2,何节玉*2

(1. 湖南理工学院 化学化工学院,湖南 岳阳  4140002. 海南热带海洋学院 海洋科技学院,海南 三亚  572022)

 

摘要:介绍了一种生物基多官能团有机酸―C22-脂环族三羧酸()的改进合成工艺,并与其相关的文献报道进行了比较。在单质碘的催化作用下,从海蓬籽油制备的共轭亚油酸与顺丁烯二酸酐进行Diels-Alder反应合成了上述产物;通过L9(34)正交试验优化了合成工艺条件;选用正庚烷为溶剂分离产物,并经FTIRMSNMR证实。正交试验得到的优化工艺条件为:顺丁烯二酸酐与共轭亚油酸的物质的量比为1.2、催化剂用量0.2 wt %、反应温度60 °C、反应时间2.0 h,此条件下产率高达96.5%。本改进合成工艺具有低温、常压、高效、产物分离相对简单等优点。

关键词:海蓬籽油;共轭亚油酸;C22-脂环族三羧酸()Diels-Alder反应;改进合成

中图分类号:O624.5     文献标识码:A      文章编号:0258-32832019--

 

Improvement on Synthesis of C22-cycloaliphatic Tricarboxylic Acid (Anhydride) LIAO De-zhong1, ZHAN Da-dong2, SUN Hong-yuan2, ZHAO Yu-ling2, HE Jie-yu2 (1. College of Chemistry & Chemical Engineering, Hunan Institute of Science & Technology, Yueyang 414000, China; 2. College of Marine Science & Technology, Hainan Tropical Ocean University, Sanya 572022, China) Huaxue Shiji, 2019, 41(  ),

Abstract: The improved synthetic process for the preparation of C22-cycloaliphatic tricarboxylic acid (anhydride), a bio-based multifunctional organic acid, was present and compared with that reported in the other publications. In order to obtain this product, Diels-Alder reaction of conjugated linoleic acid derived from salicornia herbacea seed oil with maleic anhydride, was carried out using iodine as a catalyst. An orthogonal test design L9 (34) was applied to determine the optimum condition for the preparation. The n-heptane was chosen as the solvent to separate the product which was confirmed by FTIR, MS and NMR. The optimum conditions were obtained as follow: molar ratio of maleic anhydride to conjugated linoleic acid of 1.2, dosage of catalyst of 0.2 wt % (in respect to the total mass of the reactants), reaction temperature of 60 °C and reaction time of 2.0 h; under which the yield could reach 96.5%. The improved synthetic process showed various advantages such as low-temperature, atmospheric-pressure, high-efficiency, and relatively simple product separation.

 

N-氨基磺酰基甲脒类化合物的合成研究

伍悦瑄,阿不都热合曼·乌斯曼*

(新疆师范大学 化学化工学院,新疆 乌鲁木齐 830054

 

摘要:以二氯甲烷为溶剂,甲酰胺在三氯氧磷的活化作用下生成活性中间体,再与N-氨基磺酰胺发生缩合反应生成一系列的目标化合物,并通过红外光谱(FT-IR),核磁共振(NMR)和高分辨质谱(HR-MS)等分析方法进行结构表征。讨论了卤化试剂、温度、溶剂以及反应物投料比对产率的影响。结果表明,最佳反应条件为:三氯氧磷作为卤化试剂,二氯甲烷为溶剂,nN-氨基磺酰胺):n(甲酰胺) 11.5,温度为40 ℃,目标化合物的最高产率可达到95%

关键词N-氨基磺酰脒,N-氨基磺酰胺,三氯氧磷,甲酰胺

中图分类号O626     文献标识码A     文章编号0258-32832019--

 

Synthesis of N-sulfamoyl formamidines WU Yue-xuan, ABUDUREHEMAN Wusiman* (School of Chemistry and Chemical Engineering, Xinjiang Normal University, Urumqi 830054, China) Huaxue Shiji, 2019, 41(6),

Abstract: A series of the target compounds have been efficiently synthesized through direct condensation of sulfamides and formamides in the presence of phosphorus oxychloride using dichloromethane as solvent. The structures were characterized by FT-IR, NMR, and HR-MS. The effects of activating agent, temperature, solvent and the reactants dosage on the reaction yield were studied. The results showed that the optimal reaction conditions were phosphorus oxychloride as halogenation reagent, methane dichloride as solvent, n (N-aminosulfonamide): n (formamide) 1:1.5 at 40 in dichloromethane. The highest yield of the target product was up to 95% under the optimum reaction conditions.

Key words: N-sulfamoyl formamidine; sulfamide; phosphorus oxychloride; formamide

 

木耳状g-C3N4的合成

王俊林a,张亚娜a,李梦佳a,李小妹a,常玥*a,b,查飞a

(西北师范大学 a.化学化工学院, b.生态环境相关高分子材料教育部重点实验室, 甘肃 兰州  730070)

 

摘要:以三聚氰胺、三聚氯氰为原料,550 ℃热聚合法制备了g-C3N4(FCN)13C NMRXRD证明该g-C3N4的结构单元是3-s-三嗪环。电镜照片显示FCN形貌为木耳状,边缘较厚。原料三聚氯氰、三聚氰胺分别是4 g2 g时,N2吸附-脱附测定FCN1的比表面积为156.25 m2/g,孔径60 nmUV-vis漫反射测试FCN1的吸收边缘为482 nm,对应禁带宽度2.57 eVPL光谱显示FCN1光致发光强度最弱。可见光照射下,30 mg FCN1加入30 mL30 mg/L)的罗丹明BRhB)溶液中,50 minRhB的光降解率是99.6%,光催化剂循环实验表明该木耳状g-C3N4具有良好的稳定性。

关键词:g-C3N4;木耳状;高比表面积;光催化;RhB

中图分类号:O643.36   文献标识码:A    文章编号:0258-3283(2019)--

 

Preparation of Fungus-like g-C3N4 WANG Jun-lina, ZHANG Ya-naa, LI Meng-jiaa, LI Xiao-meia, CHANG Yue*a,b, ZHA Fei a (a. College of Chemistry and Chemical Engineering, 2. Key Laboratory of Eco-environment-related Polymer Materials Ministry of Education, Northwest Normal University, Lanzhou 730070, China), Huaxue Shiji, 2019, 41(5),

Abstract: The fungus-like g-C3N4(FCN) was prepared by thermal polymerization of cyanuric chloride, melamine and deionized water at 550 oC. The tris-s-triazine units in FCN were confirmed by 13CNMR and XRD. The surface morphology of FCN was similar to a white fungus and the crimped edge was thicker. The surface area and pore size of FCN1 was 156.25 m2/g and 60 nm by N2 adsorption-desorption using 4 g cyanuric chloride and 2 g melamine as material. UV-visible DRS showed that FCN1 had band edge at ca. 482 nm corresponding to 2.57 eV. PL spectra showed that the photoluminescence intensity of FCN1 was the weakest in several materials. When 30 mg FCN1 was added in 30 mL Rhodamine B solution (30 mg/L), the decomposition rate of RhB was 99.62% after 50 min under the visible-light irradiation. The results of photocatalyst repeated experiment showed that FCN1 had good stability.

Key words: g-C3N4; fungus-like; high-surface-area; photocatalysis; RhB

 

 

硝基烯烃与丙二酸酯的Michael加成反应研究

林敬a, b,徐立杰b,范欣然b,刘兆芳b,潘婷b,戴兢陶*b

(盐城师范学院 a.分析测试中心,b.化学与环境工程学院,江苏 盐城  224007)

 

摘要:β-CF3-β-(3-吲哚)硝基烯烃衍生物和丙二酸酯为反应起始原料,在碳酸铯碱性条件下,用甲苯作为反应溶剂,于35 ℃下搅拌反应,实现了β-CF3-β-(3-吲哚)硝基烯烃衍生物与丙二酸酯的Michael加成反应。通过对碱、反应溶剂、碱的用量、底物浓度和反应温度等因素的考察,确定了反应的最优条件。然后,在最优条件下,实现了不同结构的β-CF3-β-(3-吲哚)硝基烯烃与丙二酸酯的Michael加成反应,以最高95%的收率获得了既含三氟甲基又含吲哚片段的γ-硝基丁酸酯,其结构均经过1HNMR13CNMRESI-HRMSIR确证。

关键词:β-CF3-β-(3-吲哚)硝基烯烃;丙二酸酯;Michael加成反应;γ-硝基丁酸酯

中图分类号:O626.1        文献标识码:A           文章编号:0258-32832019

 

Michael Addition Reactions of Nitroalkenes with Malonates LIN Jinga,b, XU Li-jieb, FAN Xin-ranb, LIU Zhao-fangb, PAN Tingb, DAI Jing-tao*b (a. Instrumental Analysis Center, b. School of Chemistry and Environmental Engineering, Yancheng Teachers University, Yancheng 224007, China), Huaxue Shiji, 2019, 41(4),

Abstract: In the work, the Michael addition reaction of β-CF3-β-(3-indolyl)-nitroalkene and malonate has been realized. The effects of base, solvent, amount of base, substrate concentration and temperature on the reaction were investigated and the optimal condition for the reaction was obtained. Then, under the optimal condition, Michael addition reactions of the different structure of β-CF3-β-(3-indolyl)-nitroalkenes with malonates, affording γ-nitrobutyrates containing trifluoromethyl and indole fragments in high yields (up to 95% yield). All compounds were fully confirmed by 1H NMR, 13C NMR, ESI-HRMS and IR.

Key words: β-CF3-β-(3-indolyl)-nitroalkenes; malonates; Michael addition reactions; γ-nitrobutyrates