硅球表面制备荧光印迹聚合物检测高效氟氯氰菊酯的研究
王吉祥,孙琳,汪云云,闫永胜*
(江苏大学 化学化工学院,江苏 镇江 212013)
摘要:采用沉淀聚合法制备了以高效氯氟氰菊酯(Beta-Cyhalothrin,BC)为模板分子的荧光分子印迹聚合物。甲基丙烯酸甲酯为功能单体、三羟甲基丙烷三甲基丙烯酸酯作为交联剂。通过红外光谱、紫外光谱、扫描电镜、透射电镜、热重分析证明已成功地合成荧光分子印迹聚合物微球,并且具有良好的球形形貌(微球粒径约为200 nm,印迹层厚度约为20 nm)、良好的单分散性、卓越的热稳定性。通过荧光检测实验可知,荧光强度与BC的浓度呈线性关系并建立了线性回归方程:I0/I-1 = 0.0041c-0.0186,R2 = 0.9837,检出限为13.251 nmol/L。通过选择性实验说明,荧光分子印迹聚合物对BC具有较好的特异性识别性能。
关键词:高效氯氟氰菊酯;荧光分子印迹聚合物;沉淀聚合
中图分类号:TN247 文献标识码: A 文章编号: 0258-3283(2017)
Detection of Beta-cyhalothrin by a Core-shell Spherical SiO2-based Surface Fluorescent Molecularly Imprinted Polymer WANG Ji-xiang, SUN Lin, WANG Yun-yun, YAN Yong-sheng*(School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, China), Huaxue Shiji, 2017, 39(9)
Abstract: In this work, fluorescent molecularly imprinted polymers(FMIPs) was synthesized via precipitation polymerization. Beta-cyhalothrin(BC) as the target molecule, methyl methacrylate(MMA) as the functional monomer, 3-trimethylolpropane trimethacrylate(TRIM) as the cross linker. The characteristic of material has been measured by FTIR, UV, SEM, TEM, TGA. The resulting FMIPs are monodispersed sphere(average diameter and shell thickness of as-synthesized microspheres were 200 and 20 nm), and they have good thermal stability. The FMIPs is quenched specifically by BC by fluorescence detection. The linear range describe by the Stern-Volmer equation is I0/I-1=0.0041c-0.0186, R2 = 0.9837. A lower limit of detection(LOD) is 13.251 nmol/L. It is demonstrated that high selectivity of FMIPs towards BC by selective detection.
Key words: beta-cyhalothrin; fluorescent molecularly imprinted polymers; precipitation polymerization
基于1, 8-萘酰亚胺延迟荧光材料的合成及性能研究
黄斌*1, 2,林洁1,周娜1,吴丽君1,李筱轩1,赵强1
(1. 江苏第二师范学院 生命科学与化学化工学院 江苏省生物功能分子重点实验室,江苏 南京 210013;
2. 东南大学 化学化工学院,江苏 南京 211189)
摘要:通过Suzuki交叉偶联反应得到三苯胺和N-苯基咔唑分别取代的1, 8-萘酰亚胺衍生物,化合物结构经1HNMR、质谱和元素分析表征。两种材料都是双极分子,存在分子内电荷转移,单线态-三线态能级差分别为0.40和0.32 eV。荧光量子效率和荧光寿命的测试结果表明,两种材料均能发射延迟荧光。
关键词:1, 8-萘酰亚胺;三苯胺;N-苯基咔唑;荧光;延迟荧光;双极
中图分类号:O644.19 文献标识码:A 文章编号:0258-3283(2017)
Synthesis and Properities of Delayed Fluorescence Materials Based on 1, 8-Naphthalimide HUANG Bin*1, 2, LIN Jie1, ZHOU Na1, WU Li-jun1, LI Xiao-xuan1, ZHAO Qiang1(1. Jiangsu Key Laboratory of Biological Functional Molecules, College of Life Science and Chemistry, Jiangsu Second Normal University, Nanjing 210013, China; 2. School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, China),Huaxue Shiji,2017,39(9)
Abstract: Two derivatives based on triphenylamine and N-phenyl carbazole substituted 1, 8-naphthalimide have been synthesized by Suzuki cross-coupling reactions. Structures of the target compounds are confirmed by 1HNMR, MS, and elemental analyses. The two bipolar compounds based on intramolecular charge transfer exhibit small energy gaps between singlet and triplet (ΔEST) of 0.40 and 0.32 eV, respectively. The results of fluorescent quantum yields and fluorescent lifetime indicate that two materials can emit delayed fluorescence.
Key words: 1, 8-naphthalimide; triphenylamine; N-phenyl carbazole; fluorescence; delayed fluorescence; bipolar
1-(5, 7-二羟基-2, 2-二甲基苯并吡喃)-3-(2, 2-二甲基苯并吡喃)双氢查尔酮的首次全合成
牛明杰,杨金会*,马涛,李方辉,叶子平,冯月基,严志明
(宁夏大学 化学化工学院,宁夏 银川 750021)
摘要:标题化合物是从Metrodorea stipularis树枝中提取出来的,此化合物具有抗南美洲锥虫病、抗疟疾、抗肿瘤等药理作用。以廉价的2, 4, 6-三羟基苯乙酮、对羟基苯甲醛等为原料,完成了标题化合物的全合成。所有新化合物的结构均经过NMR、IR、HR-MS确认。初步生物活性实验结果表明,对大肠杆菌的最小抑菌浓度为32 ug/mL。
关键词:吡喃环;查尔酮;全合成;抑菌
中图分类号:TQ28 文献标识码:A 文章编号:0258-3283(2017)
Total Synthesis of 1-(5, 7-Dihydroxy-2, 2-dimethylchroman-6-yl)-3-(2, 2-dimethylchrom an-6-yl)propan-1-one NIU Ming-jie, YANG Jin-hui*, MA Tao, LI Fang-hui, YE Zi-ping, FENG Yue-ji, YAN Zhi-ming(College of Chemistry and Chemical Engineering, Ningxia University, Ningxia 750021, China), Huaxue Shiji, 2017, 39(9)
Abstract:1-(5, 7-Dihydroxy-2, 2-dimethylchroman-6-yl)-3-(2, 2-dimethylchroman-6-yl)propan-1-one was isolated from stem of metrodoreastipularis. This compound had the pharmacological effect on antichagastic, antimalarial and antitumoral. Herein, 1-(5, 7-dihydroxy-2, 2-dimethylchroman-6-yl)-3-(2, 2-dimethylchroman-6-yl)propan1-one was synthesized from cheap starting material 2, 4, 6-trihydroxyacetophenonehydrate and hydroxybenzaldehyde. The structures of all new compounds were confirmed by NMR, IR and HRMS. The preliminary bioassay showed that the MIC of the compound with Esherichia coli was 32 ug/mL.
Key words:chromene; chalcone; total synthetic; antibacteria
3-氨基-1, 2-苯并-a-吡喃酮类衍生物的合成及抗氧化研究
闵曼a,丰翠b,杜俊b,任建辉b,陈琳*b
(广东药科大学 a. 中药学院,b. 药学院,广东 广州 510006)
摘要:以2, 3, 4-三甲氧基苯甲醛为原料,经4步反应合成了两个未见文献报道的含1, 2-苯并-a-吡喃酮类衍生物,其结构经NMR和MS确证。体外抗氧化性能测试结果显示,N-(7, 8-二甲氧基-3-1, 2-苯并-a-吡喃酮)苯乙酰胺在高浓度时显示出比对照品和3-氨基-7, 8-二甲氧基-1, 2-苯并-a-吡喃酮更好的DPPH自由基清除活性,在低浓度时则对羟自由基表现出比对照品及3-氨基-7, 8-二甲氧基-1, 2-苯并-a-吡喃酮更好的抑制活性,在ABTS自由基清除实验中,低浓度的3-氨基-7, 8-二甲氧基-1, 2-苯并-a-吡喃酮展现出较对照品更佳的清除活性,两者具有进一步研究的价值。
关键词:1, 2-苯并-a-吡喃酮类化合物;合成;抗氧化
中图分类号:O626.4 文献标识码:A 文章编号:0258-3283(2017)
Synthesis and Antioxidant Activity of 2H-Chromen-2-one Derivatives MIN Mana, FENG Cuib, DU Junb, REN Jian-huib, CHEN Lin*b(a. College of Traditional Chinese Medicine, b. School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006, China), Huaxue Shiji, 2017, 39(9)
Abstract: Two 2H-chromen-2-one derivatives were synthesized from 2, 3, 4-trimethoxybenzaldehyde by four steps reaction. The two compounds were synthesized and confirmed by NMR and MS. In vitro antioxidant activity test results showed that compound 5a with high concentration showed higher DPPH radical scavenging activity than control and compound 4. In a hydroxyl radical-scavenging test, compound 5a showed better inhibitory activity than control and compound 4 at low concentrations. In addition, in the ABTS free radical scavenging experiment, the low concentration of compound 4 showed better scavenging activity than the control. Therefore, both of them have the value of further research.
Key words: 2H-chromen-2-one derivatives; synthesis; antioxidant
冠醚修饰的紫精类化合物的合成与电化学性能研究
贾涛,李淼,马国丽,段中余*
(河北工业大学 化工学院,天津 300130)
摘要:将苯并氮杂-15-冠-5的边臂链接到4,4'-联吡啶上,设计合成了3种冠醚环修饰的紫精化合物。运用紫外光谱考察了其识别碱金属离子的能力,运用循环伏安测试考察了其电化学氧化还原性质。紫外光谱测试结果显示,含有两个冠醚环的紫精化合物对金属离子有较显著的配位作用。循环伏安测试结果显示,氯化1, 1'-双[ 2-酮-2-(苯并氮杂15冠5)]-4,4'-联吡啶盐化合物具有更好的电化学信号,出现了两对可逆的氧化还原峰。
关键词:冠醚;苯并-15-冠-5;紫精;电化学;循环伏安;离子识别
中图分类号:O626 文献标识码:A
Synthesis andElectrochemical Properties of Viologens Modified by Crown Ethers JIA Tao, LI Miao, MA Guo-li, DUAN Zhong-yu* (School of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130)
Abstract:Three kinds of viologens modified by crown ethers have been synthesized via the reaction of 4,4'-bipyridine with benzoaza-15-crown-5.The recognition abilities towards alkali metal ion were evaluated by UV-vis and the electrochemical redox characters were investigated using cyclic voltammetry. The result of UV-vis shows that viologen with two crown ethers has a significant coordination with alkali metal ion. The cyclic voltammetry also indicates that viologen 2 with better electrochemical signals has two pairs of reversible redox peaks.
Key words:crown ether; benzoaza-15-crown-5; viologen; electrochemistry; cyclic voltammetry; ion recognition
锶磷化膜镁基疏水膜层的构筑及其抗腐蚀性能研究
曹京宜1,张海永1,张寒露1,杨萌2,陈蓉蓉*2,王君2
(1. 91872部队海军涂料分析检测中心,北京 102442;2.哈尔滨工程大学 材料科学与化学工程学院,黑龙江 哈尔滨 150001;3. 青岛海洋新材料科技有限公司,山东 青岛 266100)
摘要:以十七氟癸基三甲氧基硅烷的无水乙醇溶液作为疏水处理液,对已覆盖锶磷化膜的镁合金样品涂层进行改性。采用扫描电子显微镜、能谱仪、静态接触角测试等方法对疏水膜层的形貌、组成及接触角等性质进行表征。采用电化学阻抗谱和动电位极化曲线对疏水膜层的耐腐蚀性能进行测定。改性后的疏水表面静态接触角值随着浸泡时间的延长而增大,其膜层表面的锶、磷和氧元素含量降低而碳元素的含量大大增加,同时也新增了硅元素。随着浸泡时间的推移,疏水性表面的耐腐蚀性有了显著的提高。
关键词:锶磷化膜;超疏水;抗腐蚀
中图分类号:TQ15 文献标识码:A 文章编号:0258-3283(2017)
Fabrication of a Hydrophobic Strontium Phosphate Film on Magnesium Alloy with Corrosion Resistance CAO Jing-yi1, ZHANG Hai-yong1, ZHANG Han-lu1, YANG Meng2, CHEN Rong-rong*2, WANG Jun2(1. 91872 Army Navy Coating Analysis and Testing Center,BeiJing 102442; 2. School of Materials Science and Chemical Engineering, Harbin Engineering University, Harbin 150001, China; 3. Qingdao Marine New Materials Technology Co., Ltd., Qingdao 266100, China), Huaxue Shiji, 2017, 39(9)
Abstract: In this work, an ethanol solution of heptadecafluorodecyl trimethoxysilane was used as the hydrophobic treatment solution to modify the coating of the magnesium alloy coated with strontium phosphating film. The morphology, composition and contact angle of the hydrophobic membrane were characterized by scanning electron microscopy, energy dispersive spectrometer and static contact angle measurement. The electrochemical impedance spectroscopy and potentiodynamic polarization curves were used to determine the corrosion resistance of the hydrophobic membrane. The static contact angle of modified hydrophobic surface was increased with the immersion time and the content of strontium, phosphorus and oxygen on the surface of the film was reduced and the content of carbon element is greatly increased, and the silicon element appeared. The hydrophobic surface of the corrosion resistance has been significantly improved after immersion.
Key words: strontium phosphate coating; superhydrophobic; corrosion resistance
单宁酸磷酸酯的合成及其抗氧化性能评价
巴丽思,王留柱,安丽萍,卫钰茹,靳利娥*
(太原理工大学 化学化工学院,山西 太原 030024)
摘要:以单宁酸为原料、三聚磷酸钠为磷酰化试剂、尿素为催化剂,进行磷酸化反应合成了单宁酸磷酸酯。通过正交试验优化最佳合成工艺并利用磷含量计算产率,并利用傅里叶红外光谱(FT-IR)、紫外光谱(UV)表征其结构。研究了单宁酸磷酸酯的电导性,并利用对羟基自由基(•OH)和超氧阴离子自由基(•O2-)的清除能力评价了抗氧化性能。结果表明,最佳合成工艺条件为n(单宁酸): n(三聚磷酸钠)= 1 : 1、反应时间为18 h、反应温度为65 ℃,在此条件下的产率可达86.02%。产物的电导率与浓度呈显著正相关,并在一定浓度下比单宁酸高出10 ~ 15倍;当质量浓度为1 g/L时,对•OH和•O2-清除率分别为75%和55%。结果证明,在优化的最佳条件下产率较高,所合成的单宁酸磷酸酯具有较好的抗氧化活性。
关键词:单宁酸;单宁酸磷酸酯;电导性;抗氧化活性
中图分类号:O629 文献标识码:A 文章编号:0258-3283(2017)
Synthesis and Antioxidant Activity in Vitro of Tannic Acid Phosphate BA Li-si , WANG Liu-zhu , AN Li-ping , WEI Yu-ru , JIN Li’e* (College of Engineering and Technology, Taiyuan University of Technology, Taiyuan,030024, China)
Abstract:Tannic acid was synthesized from tannic acid as raw material, sodium tripolyphosphate as phosphorylating reagent and urea as catalyst to phosphorylate tannic acid. The optimum synthesis process was obtainedby orthogonal test and the yield was calculated by using phosphorus content. The structure of the product was confirmedby FT-IR, and UV. The electrical conductivity of tannic acid phosphate was investigatedand the antioxidant properties were evaluated by the scavenging ability of hydroxyl radical (•OH)and superoxide anion radical(•O2-) .The results showed that the optimal synthesis conditions were n (tannic acid): n (sodium tripolyphosphate) = 1 : 1, reaction time 18 h, reaction temperature 65 ℃. Under the optimal conditions, the yield of the product was 86.02%.The conductivity of the product was positively correlated with the concentration and was 10 ~ 15 times higher than that of tannic acid at a certain concentration. When the mass concentration of 1g/L, the clearance rates of •OH and•O2- were 75% and 55%.The results showed that the yield of tannic acid phosphate was better under the optimized conditions,and the synthesized tannic acid phosphate had better antioxidant activity.
Key words:tannic acid; tannic acid phosphate; electrical conductivity; antioxidant activity
低共熔溶剂的分子结构及物性估算的研究进展
胡丽华,陈砺,方泳华,严宗诚*
(华南理工大学 化学与化工学院,广东 广州 510000)
摘要:低共熔溶剂具有熔点低、不挥发、不易燃、溶解性良好、易合成、廉价、低毒、腐蚀性低、生物降解性好等特点,常被作为“绿色”溶剂应用于金属加工和合成反应中。然而,目前对低共熔溶剂的结构和性质的研究只限于少部分具体的低共熔溶剂,没有形成系统全面的理论体系。简述了低共熔溶剂的合成与分类、分子结构和形成机理的研究进展,归纳了低共熔溶剂的物性估算方法,并指出了一些关于低共熔溶剂研究中存在的问题,提出了可能的解决方案。
关键词:低共熔溶剂;物理性质;估算
中图分类号:O645.4 文献标识码:A 文章编号: 0258-3283(2017)
Molecular Structure and Physical Property Estimation of Deep Eutectic Solvents (DESs) HU Li-hua, CHEN Li, FANG Yong-hua, YAN Zong-cheng*(School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510000, China), Huaxue Shiji, 2017, 39(9)
Abstract:The physical properties of deep eutectic solvents (DESs) have low melting point, nonvolatile, nonflammability, good solubility. And DESs are cheaper, easier to synthesize and possess lower eco-toxicity, lower corrosivity as well as favorable biodegradability, thus they have quite good potential for application in metal processing and synthesis reactions. However, the structure and properties research of DESs limited to some specific DESs, there is no a comprehensive theoretical system. In this work, the synthesis methods, classification, molecular structure, formation mechanism, and other properties of DESs were reviewed, and the estimation of physical properties were concluded. Moreover, the latent problems and probable solution about the research of DESs are discussed.
Key words:deep eutectic solvents; physical properties; estimation
化学发光试剂的研究新进展
庞彬彬,孙海鹰,徐云根*
(中国药科大学 药学院,江苏 南京 210009)
摘要:文章综述了近五年几种主要化学发光试剂的最新研究进展,内容涉及鲁米诺类、吖啶酯类、1, 2-二氧杂环丁烷类及过氧草酸酯类这4类化学发光试剂的概述及其新型衍生物的相关介绍。
关键词:化学发光试剂;研究进展;新型衍生物
中图分类号:O664.17 文献标识码:A 文章编号:0258-3283(2017)
New Progress of Chemiluminescence Reagents PANG Bin-bin, SUN Hai-ying, XU Yun-gen* (School of Pharmacy, China Pharmaceutical University, Nanjing 210009, China), Huaxue Shiji, 2017, 39(10)
Abstract: The progress of some chemiluminescence reagents in recent five years was reviewed. It consisted of the summary and introduction of the new derivatives of luminol, acridinium ester, 1, 2 -dioxetanes and peroxyoxalate.
Key words: chemiluminescence reagents; development; new derivatives
血清中钠离子检测的量值溯源性研究
吴永明,陶武*,钟广蓉,黄飞雪,廖丽红
(北京科技大学 化学分析中心,北京 100083)
摘要:首先建立了血清钠检测的量值溯源流程系统,将厂商提供的校准品溯源至参考物质和参考方法,其中参考方法选用IFCC推荐的火焰原子发射光谱法(FAES)。根据EP9-A2要求,用临床检测的常规方法与参考方法同时测定49例血清样本,进行对比实验。完成了血清钠离子产品校准品的量值溯源,建立了血清钠离子检测系统的量值溯源性,以提高检测结果的可靠性。实验结果显示,临床检测的常规方法和参考方法有很好的相关性,且两种方法的测值偏差符合CLIA′88的要求。
关键词:钠;原子吸收分光光度法;参考物质;参考方法;量值溯源
中图分类号:R446 文献标识码:A 文章编号:0258-3283(2017)
Traceability Research on Magnitude of Serum Sodium Ion WU Yong-ming, TAO Wu*, ZHONG Guang-rong, HUANG Fei-xue, LIAO Li-hong(Center of Chemical Analysis, University of Science and Technology, Beijing 100083, China), Huaxue Shiji, 2017, 39(9)
Abstract: The system of magnitude traceability of serum sodium ion was created. The calibration from the manufacturers trace to the reference material and reference method. Flame atomic emission spectrometry (FAES) which recommended by IFCC was applied to the reference method. Based on the requirements of EP9-A2, 49 cases of serum samples were determined by routine methods and reference methods. In this work, the traceability of the magnitude of the serum sodium ion product calibration was completed, and the traceability of the value of the serum sodium ion detection system was established to improve the reliability of the test results. The experimental results show that there was a good correlation between the conventional method and the reference method, and the deviation of the two methods was in accordance with the requirements of CLIA′88.
Key words: sodium; flame atomic emission spectrometry; reference material; reference method; traceability
洗手液中三氯生含量的测定方法
侯悦a,陈建秋b,陈锦芳a,沈卫阳* a
(中国药科大学 a. 理学院,b. 工学院,江苏 南京 211198)
摘要:建立盐辅助超声提取、高效液相色谱法测定洗手液中三氯生含量的方法。在硫酸铵条件下,以乙腈为提取剂,超声提取洗手液中的三氯生,并用高效液相色谱仪进行测定。在0.1 ~ 20 µg/mL浓度范围内,三氯生峰面积与其浓度呈良好的线性关系。三氯生的检出限(S/N = 3)为0.02 µg/mL,加标回收率在94.6% ~ 97.3%之间,相对标准偏差为3.69%。该方法经济简便、重复性好,可用于测定洗手液中三氯生的含量。
关键词:三氯生;洗手液;盐;超声;高效液相色谱
中图分类号:O657.7 文献标识码:A 文章编号:0258-3283(2017)
Determination Method of Triclosan in Hand Sanitizer HOU Yuea, CHEN Jian-qiub, CHEN Jin-fanga, SHEN Wei-yang*a( a. College of Science, b. Institute of Technology, China Medical University, Nanjing 211198, China), Huaxue Shiji, 2017, 39(9)
Abstract: The analytical method for determination of triclosan in hand sanitizer was established with ultrasound-assisted salt-induced extraction and high performance liquid chromatography (HPLC). In the presence of ammonium sulfate, triclosan was ultrasonically extracted with acetonitrile and determined by high performance liquid chromatography. Detection was liner in the concentration range of 0.1 ~ 20 μg/mL and limit of detection (S/N = 3) was 0.02 μg/mL. The spiked recoveries were 94.6% ~ 97.3% and the relative standard deviation of triclosan was 3.69%. The method is inexpensive and easy with high accuracy and precision. It can be used to determine triclosan in hand sanitizer.
Key words: triclosan; hand lotion; salt; ultrasonic; high performance liquid chromatography
三氯卡班的波谱学数据与结构确证
李永利,姜阳,李杰*,许卓妮,陈鹰
(上海市计量测试技术研究院,上海 201203)
摘要:建立了一种仪器分析技术确证三氯卡班化学结构的方法。采用紫外光谱、红外光谱、高分辨质谱、核磁共振、热重分析、差示扫描量热法和单晶X-射线衍射法对三氯卡班进行结构表征。通过对紫外和红外光谱的特征峰解析,1HNMR和 13CNMR谱信号详细归属,热分析(TGA/DSC)结果解析以及X-射线衍射技术证明,最终确证了三氯卡班的分子结构。
关键词:波谱学;三氯卡班;核磁共振;结构确证
中图分类号:O657 文献标识码:A 文章编号:0258-3283(2017)
Spectral Analysis and Structural Identification of Triclocarban LI Yong-li, Jiang Yang, LI Jie*, XU Zhuo-ni, CHEN Ying (Shanghai Institute of Measurement and Testing Technology, Shanghai 201203, China)
Abstract:A determinationmethod for the chemical structure oftriclocarban was established.The structure was elucidated by UV, IR, HR-MS, NMR, TGA, DSC, and X-ray diffraction analysis. The UV and IR absorption peaks were discussed, and all the signals of 1HNMR and 13CNMR were attributed to the respective positions in the molecule. The test result of TGA/DSC was analyzed, and the molecular structure was determined by X-ray crystallography finally.
Key words: spectroscopy; triclocarban; nuclear magnetic resonance; structural identification
柱切换离子色谱法测海水中的草酸根离子
沈燕飞,吴琪琪,林智威,陈一帆,陈梅兰*
(浙江树人大学 生物与环境工程学院,浙江 杭州 310015)
摘要:建立了柱切换离子色谱法测海水中草酸根离子的方法。采用Dionex IonPac AS11-HC(4 mm×250 mm)阴离子分离柱和AG11-HC(4 mm×50 mm)保护柱分离海水中草酸根,采用20 mmol/L KOH淋洗液,流速为1.0 mL/min等度淋洗,通过柱切换除去海水中大部分的高浓度阴离子(Cl-、SO42-和Br-),分离出的C2O42-收集于富集柱,然后经过阀切换,将目标离子从富集柱上洗脱,进入阴离子分析柱Dionex IonPac AS19(4 mm×250 mm)分离,此时淋洗液换成30 mmol/L NaOH淋洗液,流速为0.8 mL/min等度淋洗,电导法检测。结果表明,在线性范围为0.1 ~ 10.0 mg/L内其相关系数为0.9994,相对标准偏差为1.48%,所得样品回收率为110.0% ~ 85.3%。该实验方法简单方便,且具有较好的重现性和较低的检出限,可用于检测海水中的草酸根离子。
关键词:柱切换;离子色谱;海水;草酸根离子
中图分类号:O657.7 文献标识码:A 文章编号:0258-3283(2017)
Determination of Oxalate in Seawater Using Ion Chromatography Couple of Column Switching Technique SHEN Yan-fei, WU Qi-qi, LIN Zhi-wei, CHEN Yi-fan, CHEN Mei-lan*(College of Biology and Environmental Engineering, Zhejiang Shuren University, Hangzhou 310015, China), Huaxue Shiji, 2017, 39(9)
Abstract: A method for determination of oxalate in seawater by ion chromatography coupe of column switching was established. Sample separation method was as follows: firstly, seawater was injected on an analytical column (Dionex Ion Pac AS11-HC,4 mm×250 mm)and a guard column (AG11-HC,4 mm×50 mm), the elution was 20 mmol/L KOH at a 1.0 ml/L flow rate. Secondly, high concentration anions ( Cl-, SO42-, and Br-) and matrix in seawater were removed by setting an appropriate valve switching time, while the C2O42- was collected a concentrator column. Thirdly, the C2O42- in concentrator was eluted on a Dionex Ion Pac AS19(4 mm×50 mm)and a AS19(4 mm×250 mm)column by another valve switching, the elution was 30 mmol/L NaOH at a 0.8 ml/L flow rate. Finally, the C2O42- was separated by chosen column and detected using conductivity detection. Under the separation conditions, the method showed good linearity (r = 0.9994) in the range of 0.1 ~ 5.0 mg/L and satisfactory repeatability (RSD < 1.48%, n = 6). The limit of detection was 4.35 µg/L (S/N = 3). The utilization of the method was demonstrated by the analysis of seawater, with satisfactory spiked recoveries of ammonium between 110.0% and 85.3%. The result showed that the single pump column-switching system was convenient and practical for the determination of low level.
Key words:column switching;ion chromatography;seawater;oxalate
胆汁酸溶解度的测定与数据关联
张佳琦a,胡祥正*b
(天津科技大学 a. 食品工程与生物技术学院,b. 化工与材料学院,天津 300457)
摘要:在胆汁酸结晶过程中,温度对胆汁酸在不同有机溶剂中溶解度的影响至关重要。采用平衡法结合HPLC法测定303.15 ~ 353.15 K内胆酸、鹅去氧胆酸、熊去氧胆酸在5种有机溶剂中的溶解度,分别采用多项式经验方程和理想溶液方程对实验数据进行关联。结果表明,胆酸、鹅去氧胆酸、熊去氧胆酸在不同有机溶剂中的溶解度均随温度升高而增加,这两种方程均能较好地关联溶解度实验数据,其中多项式经验方程关联的相关系数均在0.98以上。
关键词:胆酸;鹅去氧胆酸;熊去氧胆酸;溶解度;温度;关联
中图分类号:O621.2 文献标识码:A 文章编号:0258-3283(2017)
Determination and Correlation of the Solubility of Bile Acids ZHANG Jia-qia, HU Xiang-zheng*b(a. College of Food Engineering and Biotechnology, b. College of Chemical Engineering and Material Science, Tianjin University of Science and Technology, Tianjin 300457, China), Huaxue Shiji, 2017, 39(9)
Abstract: In the crystallization process of bile acids, temperature was of vital importance for the solubility of bile acid in different organic solvents. Equilibrium method and HPLC method were combined to determine the solubility of cholic acid, chenodeoxycholic acid, and ursodeoxycholic acid in five kinds of organic solvents in the temperature of 303.15 ~ 353.15 K. The experimental data was correlated using polynomial empirical equation and ideal solution equations. The results showed that the solubility of cholic acid, chenodeoxycholic acid and ursodeoxycholic acid in different organic solvents all increased with temperature increasing. Furthermore, the two equations could both show a better correlation of solubility test data, with the correlation coefficient of polynomial empirical equation correlation above 0.98.
Key words: cholic acid; chenodeoxycholic acid; ursodeoxycholic acid; solubility; temperature; correlation
抗风湿类中成药“骨节灵”中醋酸地塞米松和
醋酸泼尼松的快速筛查方法研究
彭梦侠*,陈妙如,余永刚,张慧玲
(嘉应学院 化学与环境学院,广东 梅州 514015)
摘要:对抗风湿类中成药“骨节灵”中是否非法添加醋酸地塞米松和醋酸泼尼松的快速筛查方法进行了研究。以抗风湿类中成药-骨节灵为研究对象,用衰减全反射附件(ATR)采集研究样品的红外光谱(FT-IR),采用Discriminant Analysis建立了单一检测是否添加醋酸地塞米松的模型、单一检测是否添加醋酸泼尼松的模型、同时检测是否添加醋酸地塞米松、醋酸泼尼松的模型。3个模型的性能指数均大于90%,稳定性良好。分别用3个模型检测了40个样品,前两种模型的正确识别率为100%,后一种模型的正确识别率稍低(95%)。
关键词:红外光谱;快速筛查;醋酸地塞米松;醋酸泼尼松;骨节灵
中图分类号:O657.33 文献标识码:A 文章编号:0258-3283(2017)
Rapid Screening of Dexamethasone Acetate and Prednisone in Chinese Medicine "Gujieling" PENG Meng-xia*, CHEN Miao-ru, YU Yong-gang, ZHANG Hui-ling(School of Chemistry and Environment, Jiaying University, Meizhou 514015, China), Huaxue Shiji, 2017, 39(9)
Abstract: Rapid screening of dexamethasone acetate and prednisone were investigated in anti-rheumatic Chinese medicine "Gujieling". Taking anti-rheumatic medicine "Gujieling" as the object, the three recognition models were established using ATR-FTIR combined with discriminant analysis, namely, model 1 detection dexamethasone acetate model, model 2 detection prednisone model, and model 3 detection dexamethasone acetate and prednisone model. The performance index of three models was greater than 90%, good stability. Three models were used to detect the 40 samples, the correct recognition rate of model 1 and model 2 was 100%, the correct recognition rate of model 3 was 95%.
Key words: ATR-FTIR; rapid screening; dexamethasone acetate; prednisone; Gujieling
城市垃圾污染监测用二氧化碳中甲烷气体标准物质的研制
李佳*1,2,宋笑明1
(1.河南省计量科学研究院,河南 郑州 450008;2. 郑州大学 材料科学与工程学院,河南 郑州 450001)
摘要:城市垃圾填埋法由于会释放大量二氧化碳和甲烷温室气体而受到广泛关注。研制了城市垃圾污染检测用气体标准物质,该标准物质以垃圾场填埋气为背景气,避免了影响填埋场释放的甲烷及二氧化碳气体检测结果的基体效应。同时还可以模拟不同环境下的垃圾场填埋气,确保城市垃圾污染监测用气体分析仪器监测数据的准确性。采用称量法制备了一系列浓度为1% ~ 65%(mol/mol)二氧化碳中甲烷气体标准物质,并对该气体标准物质的均匀性、稳定性及随压力变化的实验结果进行了分析与考察。结果表明,研制的气体标准物质量值准确,均匀性、稳定性好,已批准为国家二级标准物质 GBW(E)061757。
关键词: 甲烷;二氧化碳;填埋气
中图分类号:X831 文献标识码:A 文章编号:0258-3283(2017)
Methane in Carbon Dioxide Gas Reference Materialsfor Used in Municipal Solid Waste Pollution Monitoring LI Jia*1,2, SONG Xiao-ming1(1.Henan Institute of Metrology, Zhengzhou 450008, China;2. School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450001, China)
Abstract:Municipal solid waste pollution due to the release of carbon dioxide and methane emissions of greenhouse gases has been widely concerned. In this work, a gas reference material for monitoring of municipal solid waste is developed, which is based on the landfill gas as the background gas, which avoids the matrix effect and affects the gas standard material of methane and carbon dioxide gas monitoring results. The gas standard material can simulate landfill gas under different environmental conditions, and ensure the accuracy of the instrument monitoring data analysis.This workwas prepared by gravimetric method for a series of methane in carbon dioxide gas reference materials, which concentration range is 1% ~ 65% (mol/mol), and the uniformity, stability and the concentration variation as the pressure changing were investigated. The experimental results show that gas standard material developed quality value accurate, good uniformity and stability, which can fulfill requirements of warrant reference materials absolutely.
Key words:methane;carbon dioxide;landfill gas
恩诺沙星纯度标准物质的定量核磁定值研究
及其不确定度评估
刘芳,张丽媛,王敏*,杨梦瑞,周剑,王彤彤
(中国农业科学院农业质量标准与检测技术研究所农业部农产品质量安全重点实验室,北京100081)
摘要:采用定量核磁法对恩诺沙星标准物质进行纯度定值研究,考察了定量核磁中选择不同定量峰的定值结果,并系统评估了定量核磁法引入的定值不确定度。同时采用质量平衡法对恩诺沙星纯度进行定值。结果表明,恩诺沙星纯度标准物质核磁定值结果为99.7%,核磁定值不确定度为0.5%。
关键词:恩诺沙星;标准物质;定量核磁;不确定度
中图分类号:O652.1 文献标识码:A 文章编号:0258-3283(2017)
Characterization and Uncertainty Evaluation of Enrofloxacin by Quantitative NMRLIU Fang, ZHANG Li-yuan, WANG Min*, YANG Meng-rui, ZHOU Jian, WANG Tong-tong(Key laboratory of Quality and Safety of Agro-products of Ministry of Agriculture, Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agriculture, Beijing100081, China)
Abstract:The quantitative NMR was employed to measure the mass fraction of enrofloxacin and the measurement uncertainty was systematically evaluated. The influence of assigned quantitative peaks on pirity determination was discussed. Additionally, mass balance method was applied to measure the purity of enrofloxacin. The mass fraction of enrofloxacin determined by qNMR was 99.7%, and the characterization uncertainty of qNMR was 0.5%.
Keywords: enrofloxacin; certified reference material;qNMR; uncertainty
氮掺杂碳纳米粒子荧光共振能量转移测定核黄素
张士超,林晨韵,黄浩,郭嘉庆,黄庭庭,冼嘉琪,翁文*
(闽南师范大学 化学与环境学院,福建 漳州 363000)
摘要:以柠檬酸和乙二胺为前驱体,在油酸介质中通过微波辅助法一步合成了氮掺杂荧光碳纳米粒子,量子产率达41.5%。碳纳米粒子与核黄素可发生有效的荧光共振能量转移,基于此建立了一种定量测定核黄素含量的新方法。测定核黄素含量的线性范围为0 ~ 20 μg/mL,检出限为68.5 ng/mL。该方法简单、快速、灵敏度高,可应用于实际样品中核黄素含量的测定。
关键词:荧光共振能量转移;氮掺杂碳纳米粒子;核黄素;乙二胺;柠檬酸
中图分类号:O657 文献标识码:A 文章编号:0258-3283(2017)
Fabrication of Nitrogen-doped Carbon Nanoparticles and Application in the Detection of Riboflavin Based on Fluorescence Resonance Energy Transfer ZHANG Shi-chao, LIN Chen-yun, HUANG Hao, GUO Jia-qing, HUANG Ting-ting, XIAN Jia-qi, WENG Wen*(College of Chemistry and Environment, Minnan Normal University, Zhangzhou 363000, China), Huaxue Shiji, 2017, 39(9)
Abstract: Nitrogen-doped carbon nanoparticles (N-CNPs) with a fluorescence quantum yield of 41.5% were prepared from ethylenediamine and citric acid in oleic acid medium by a facile microwave-assisted solvothermal method. A new approach for quick and sensitive determination of riboflavinin was developed based on fluorescence resonance energy transfer from N-CNPs to riboflavinin. There exists a good linear correlation between fluorescence signal and the concentration of riboflavin in the range of 1 ~ 20 μg/mL. The limit of detection (LOD) was estimated to be 68.5 ng/mL based on three times the standard deviation rule. This method can be applied to the determination of riboflavin in real samples.
Key words: fluorescence resonance energy transfer; nitrogen-doped carbon nanoparticles; riboflavin; ethylenediamine; citric acid
席夫碱钼(VI)配合物催化合成环氧环己烷
孙士淇a,移永杰a,常玥*a, b,査飞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:以合成的水杨醛缩2-氨甲基吡啶席夫碱钼配合物([MoO2(L1)(EtOH)])、邻羟基苯乙酮缩2-氨甲基吡啶席夫碱钼配合物([MoO2(L2)(EtOH)2])、2-吡啶甲醛缩邻氨基酚席夫碱钼配合物([MoO2(L3)(EtOH)])为催化剂,研究了叔丁基过氧化氢(TBHP)作氧化剂,3种配合物在制备环氧环己烷中的催化活性。详细考察了反应时间、温度、催化剂用量、氧化剂用量对环己烯转化率、环氧产物选择性的影响,筛选出了席夫碱钼催化剂最佳的反应条件:70 ℃,10 mg 2-吡啶甲醛缩邻氨基酚席夫碱钼配合物,n(环己烯)︰n(叔丁基过氧化氢) = 1︰2,反应5 h,环己烯的转化率为77.2%,环氧环己烷选择性>99%,产率为77.2%。催化剂重复实验表明该席夫碱配合物具有较高的稳定性。
关键词: 席夫碱;叔丁基过氧化氢;环氧环己烷
中图分类号:O643.36 文献标识码:A 文章编号:0258-3283(2017)
Catalytic Synthesis of Cyclohexene Oxideby Schiff-base Molybdenum(VI) Complex SUN Shi-qia, YI Yong-jiea, CHANG Yue*a, b, ZHA Feia(a. College of Chemistry & Chemical Engineering,b. Key Laboratory of Eco-Environment-Related Polymer Materials Ministry of Education, Lanzhou 730070,China), Huaxue Shiji, 2017, 39(9)
Abstract: The catalytic activity of three Schiff-base molybdenum(VI) complexes was investigated using tert-butyl hydroperoxide as oxidizer to synthesize epoxy cyclohexane. The complexes were characterized by means of FT-IR, elemental analysis and ICP. The catalytic activity of 2-pyridinecarboxaldehyde o-aminophenol Schiff-base molybdenum(VI) complex is the highest in three Schiff-base complexes. The influence of reaction factors containing the reaction temperature, reaction time, catalyst dosage, cyclohexene and oxidant molar ratio on the conversion of cyclohexene and selectivity of epoxy cyclohexane is investigated. At 70 ℃, molar ratio of cyclohexene to tert-butyl hydroperoxide 1 : 2, catalyst dosage10 mg and reaction time 5 h, the conversion of cyclohexene is 77.2% and the selectivity of epoxy cyclohexane is > 99%. This catalyst show high stability via run test.
Keywords:Schiff-base; tert-butyl hydroperoxide; epoxy cyclohexane
三氟甘露糖细菌内毒素检查方法的研究
冯苗,于菁菁,尹长峰,王巍*
(原子高科股份有限公司,北京 102413)
摘要:依照《中国药典(2015年版第4部)》1143细菌内毒素检查法,用不同厂家的鲎试剂对3批三氟甘露糖进行干扰试验,建立了三氟甘露糖的细菌内毒素检查方法。以无水乙腈溶解三氟甘露糖,当用细菌内毒素检查用水稀释至浓度不超过1 mg/mL时,细菌内毒素检查显示无干扰作用。建立的细菌内毒素检查方法适用于三氟甘露糖,其细菌内毒素限值为1 EU/mg。
关键词:三氟甘露糖;细菌内毒素检查;干扰试验;无水乙腈
中图分类号:TQ463 文献标识码:A 文章编号:0258-3283(2017)
Bacterial Endotoxin Test of Mannose Triflate FENG Miao, YU Jing- jing, YIN Chang-feng, WANG Wei *(HTA CO..LTD., Beijing 102413,China)
Abstract:To establish a method for the bacterial endotoxin test of mannose triflate in the FDG kit. The interference experiment for 3 batches of mannose triflate was carried out based on the general principle 1143 in Vol. Ⅳ of the 2015 version of Chinese Pharmacopoeia. Mannose triflate was dissolved with anhydrous acetonitrile and then diluted by BET water. The interference disappeared when the concentration of sample was less than or equal to 1 mg/mL. The established bacterial endotoxin test is feasible to mannose triflate. The bacterial endotoxin limit of mannose triflate is 1 EU/mg.
Key words:mannose triflate;bacterial endotoxin test;interference test;anhydrous acetonitrile
3, 4, 5-三氟-2-甲基苯类液晶化合物的合成与性能
田会强
(北京八亿时空液晶科技股份有限公司 液晶材料分析及应用技术北京市重点实验室,北京 102205)
摘要:以3, 4, 5-三氟苯酚、3, 5-二氟-4′-烷基联苯为原料,经酚羟基保护反应、丁基锂/碘甲烷上甲基反应、Williamson醚化反应等5步反应最终合成4-[二氟(3, 4, 5-三氟-2-甲基-苯氧基)甲基]-3, 5-二氟-4′-烷基联苯类化合物。纯化后目标产物的气相色谱纯度≥99.5%,总收率约为47%,结构经1HNMR及GC-MS确证。其中,合成2-(3, 4, 5-三氟-2-甲基-苯氧基)四氢吡喃采用1.2倍丁基锂为锂化试剂,3, 4, 5-三氟-2-甲基苯酚和4-溴二氟甲基-3, 5-二氟-4’-烷基联苯醚化反应的最优化条件为在DMSO中反应4 h。将该化合物添加到液晶的基础配方中,能降低旋转粘度(γ1),提高液晶的响应速度,增加介电各向异性(Δε),降低阈值电压。
关键词:4-[二氟(3, 4, 5-三氟-2-甲基-苯氧基)甲基]-3, 5-二氟-4'-烷基联苯;3, 4, 5-三氟-2-甲基苯酚;光电性能;液晶化合物
中图分类号:O753;O625 文献标识码:A 文章编号:0258-3283(2017)
Synthesis and Properties of Liquid Crystal Compound Containing 3, 4, 5-Trifluoro-2-methyl-benzene TIAN Hui-qiang(Beijing Key Laboratory of Liquid Crystal Materials Analysis and Application Technology, Beijing Bayi Space Liquid Crystal Material Technology Company, Beijing 102205, China), Huaxue Shiji, 2017, 39(9)
Abstract: 4-[Difluoro-(3, 4, 5-trifluoro-2-methyl-phenoxy)-methyl]-3, 5-difluoro-4'-alkyl-biphenylderivative was synthesized via phenolic hydroxyl protection, butyl lithium/methyl iodide methylation, and Williamson etherification reaction (five steps′ reaction) by employing 3, 4, 5-trifluoro-phenol and 3, 5-difluoro-4'-alkyl-biphenyl as starting materials. After purification processing, the total yield was 47% with the purity was 99.5% (GC), the structure was confirmed by 1HNMR and GC-MS. For the methylation reaction, 1.2 equivalents of butyl lithium was employed as lithium reagent. The optimum reaction time and solvent for etherification of 3, 4, 5-trifluoro-2-methyl-phenol with 4-(bromo-difluoro-methyl)-3, 5-difluoro-4'-methyl-biphenyl were 4 h and DMSO, respectively. The addition of the compound into the basic formula of liquid crystal not only could reduce the rotational viscosity (γ1), and the response time could be improved, as well as the dielectric anisotropy (Δε) could be improved, and threshold voltage could be reduced.
Key words: 4-[difluoro-(3, 4, 5-trifluoro-2-methyl-phenoxy)-methyl]-3, 5-difluoro-4'-alkyl-biphenyl; 3, 4, 5-trifluoro-2-methyl-phenol; electro-optical property; liquid crystal compound
新型HIV-1蛋白酶抑制剂的合成
赵松峰,张晓,师秀琴,王存良,杨志衡,张晓坚*
(郑州大学第一附属医院,河南 郑州 450052)
摘要:以Darunavir为先导化合物,运用骨架跃迁和拼合等药物设计策略,设计合成了3个结构新颖的化合物,均未见文献报道,目标化合物经1HNMR、13CNMR和MS确证。
关键词:AIDS;HIV-1 PR;合成;抑制剂;骨架跃迁
中图分类号:R914.5 文献标识码:A 文章编号:0258-3283(2017)
Synthesis of Novel HIV-1 Protease Inhibitors ZHAO Song-feng, ZHANG Xiao, SHI Xiu-qin, WANG Cun-liang, YANG Zhi-heng, ZHANG Xiao-jian*(The First Affiliated Hospital of Zhengzhou University, Zhenzhou 450052, China)
Abstract:Three new compounds were synthesized using compound Darunavir as the maincompound based on the drug design principle of scaffold-hopping and combination. All the compounds are unreported in literatures, and the structures were confirmed by 1HNMR, 13CNMR and MS.
Key words: AIDS; HIV-1 protease; synthesis; inhibitor; scaffold-hopping
脱水磷酰氯法合成磷酸二异辛酯
张辉,李效军*
(河北工业大学 化工学院,天津 300130)
摘要:研究了脱水磷酰氯法合成磷酸二异辛酯的新方法。先以五氧化二磷和二氯亚砜反应制备了脱水磷酰氯,脱水磷酰氯再与异辛醇反应制得目标产物磷酸二异辛酯。考察了磷酰氯与异辛醇物质的量比、异辛醇的滴加温度、反应时间、反应温度和真空度等关键因素对反应的影响。实验结果表明,n(脱水磷酰氯) : n (异辛醇) = 1.0 : 2.1、15 ℃下滴加异辛醇、60 ℃下反应3 h、真空度为0.08 MPa的条件下,磷酸二异辛酯的收率达96.2%,含量达97.9%。经FT-IR和NMR对产物磷酸二异辛酯进行表征。
关键词:磷酸二异辛酯;脱水磷酰氯;异辛醇;合成
中图分类号:TQ265.14 文献标识码:A 文章编号:0258-3283(2017)
Synthesis of Diisooctyl Phosphate from Phosphenic Chloride ZHANG Hui, LI Xiao-jun*(School of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130, China), Huaxue Shiji, 2017, 39(9)
Abstract:A novel process for the preparation of diisooctyl phosphate from phosphenic chloride was developed. Phosphenic chloride was synthesized from phosphorus pentoxide and thionyl chloride. Reaction of phosphenic chloride and isooctanol formed diisooctyl phosphate. The effects of key factors such as molecular ratio, dropping temperature of isooctanol, reaction time, reaction temperature and pressure on the reaction were investigated. The results indicated that under the optimal reaction conditions, n(phosphenic chloride) : n(isooctanol) was 1 : 2.1, isooctanol was dropped at 15 ℃, reaction time was 3 h at 60 ℃,and pressure was 0.08 MPa, the yield of diisooctyl phosphate was 96.2% with a purity of 97.9%. The product diisooctyl phosphate was confirmed by FT-IR and NMR.
Key words:diisooctyl phosphate; phosphenic chloride; isooctanol; synthesis
偶氮苯水杨醛缩氨基芴席夫碱的合成与表征
万屏南,崔汉峰,刘文琴,樊浩,付琪,林艳*
(江西中医药大学 药学院,江西 南昌 330004)
摘要:以苯胺和取代苯胺为原料,经重氮化、亲电取代以及缩合反应,设计合成了4种新型结构的偶氮苯水杨醛氨基芴席夫碱。利用1HNMR、13CNMR和元素分析对目标化合物的结构进行了表征。
关键词: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(2017)
Synthesis and Characterization of Azobenzene Salicylaldehyde Schiff Base Containing 2-Aminofluorene WAN Ping-nan, CUI Han-feng, LIU Wen-qin, FAN Hao, FU Qi, LIN Yan*(School of Pharmacy, Jiangxi University of Traditional Chinese Medicine, Nanchang 330004, China), Huaxue Shiji, 2017, 39(9)
Abstract: A series of novel azobenzene salicylaldehyde Schiff base containing 2-aminofluorene were synthesized by diazotization, electrophilic substitution and condensation reaction using aniline and substituted aniline as starting materials. The structure of the target product was confirmed by 1HNMR, 13CNMR and elemental analysis.
Key words: azobenzene; salicylaldehyde; Schiff base; synthesis
碘催化Gröebke反应合成3-氨基咪唑并[1, 2-a]吡啶衍生物
黄一波*1a, 2,叶爱英1b,徐瑾1a
(1. 常州工程职业技术学院 a. 制药与环境工程学院,b. 人事处,江苏 常州 213164;
2. 江苏省生物酶工程技术研究开发中心,江苏 常州 213164)
摘要:以芳香醛、2-氨基吡啶和异腈为原料,10 mol%分子碘作催化剂,甲醇作溶剂,回流反应3 h合成标题化合物。该反应条件温和,所得产物收率为76% ~ 90%。
关键词:碘催化;Gröebke反应;异腈
中图分类号:O62;O69 文献标识码:A 文章编号:0258-3283(2017)
Synthesis of 3-Aminoimidazo[1, 2-a]pyridine Derivatives Catalyzed by Iodine via Gröebke Reaction HUANG Yi-bo*1a, 2, YE Ai-ying1b, XU Jin1a(1. Changzhou Vocational Institute of Engineering, a. School of Pharmaceutical and Environmental Engineering, b. The Personnel Department, Changzhou 213164, China;2. Jiangsu Provincial Biological Enzyme Engineering Technology and Development Cente, Changzhou 213164, China), Huaxue Shiji, 2017, 39(9)
Abstract: 3-Aminoimidazo[1, 2-a]pyridine derivatives have been synthesized via one-pot method with aromatic aldehyde, 2-aminopyridine and isocyanide, using methanol as solvent, 10 mol% iodine as catalyst in relux. The reaction condition is mild, and the corresponding yields are among 76% ~ 90%.
Key words: iodine catalysis; Gröebke reaction; isocyanide
3,3’,4,4’-联苯四甲酸二酐的合成研究
吴孝兰
(国药集团化学试剂有限公司,上海 200002)
摘要:以4-氯-邻苯二甲酸酐为原料,经过酯化、偶联、水解、脱水合成3,3’,4,4’-联苯四甲酸二酐。目标产物须保存在真空干燥箱中,防止水分侵入。通过改进工艺路线,可得到高收率、高纯度的目标产物,使工业化生产成为可能,为全芳香族聚酰亚胺的生产提供高质量原料。
关键词:3,3,4,4’-联苯四甲酸二酐;4-氯-邻苯二甲酸酐;酯化;偶联;水解;脱水
中图分类号:O621.3 文献标识码:A 文章编号:0258-3283(201*)
Synthesis of 3,3,4,4’-Biphenyltetracarboxylic WU Xiao-lan (Sinopharm Chemical Reagent Co., Ltd, Shanghai 200002, China)
Abstract: This work introduces the synthesis of 3,3’,4,4’-biphenyltetracarboxylic which using 4-chlorophthalic anhydride as the raw material.3,3’,4,4’-Biphenyltetracarboxylic is synthesized by esterification, coupling, hydrolysis and dehydration. The target product shall be stored in a vacuum oven to prevent ingress of moisture. The high yield and high purity of 3,3’,4,4’-biphenyltetracarboxyliccan be obtained. Thus, the industrialized production is possible. The synthetic product can provide high quality raw materials for the production of wholly aromatic polyimide.
Key words: 3,3’,4,4’-biphenyltetracarboxylic; 4-chlorophthalic anhydride; esterification,coupling; hydrolysis; dehydration
顺式-1, 2-环戊二胺盐酸盐的合成
王建塔,李毅,李永,朱桃,樊玲玲*
(贵州医科大学 药学院,贵州 贵阳 550004)
摘要:以环戊烯为起始原料,先后经高锰酸钾氧化、甲磺酰化、胺化、氢化还原共4步反应制得目标产物,并通过1HNMR、13CNMR、ESI-MS对其结构进行了确证。该方法原料简单易得、合成路线短、反应条件温和、制备方法成熟,总收率为46.7%,是经济价值较高的合成路线。
关键词:顺式-1, 2-环戊二胺;合成;胺化
中图分类号:O629 文献标识码:A 文章编号:0258-3283(2017)
Synthesis of cis-1, 2-Cyclopentyl Amine Hydrochloride WANG Jian-ta, LI Yi, LI Yong, ZHU Tao, FAN Ling-ling* (College of Pharmacy, Guizhou Medical University, Guiyang 550004, China), Huaxue Shiji, 2017, 39(9)
Abstract: cis-1, 2-Cyclopentyl amine hydrochloride was synthesized in 46.7% overall yield from cyclopentene via potassium permanganate oxidation, mesylation, amination and hydrogenation. The structure was confirmed by 1HNMR, 13CNMR and ESI-MS. The current method has the advantages of raw material economy, short synthetic route, mild reaction conditions, simple operation and high overall yield. Thus, it is the high economic value of synthetic routes.
Key words: cis-1, 2-cyclopentyl amine; synthesis; amination
2-碘-3-溴-5-氯吡啶的合成
赵春深*,李廷涛,周志旭,刘强,王明扬
(贵州大学 药学院,贵州 贵阳 550003)
摘要:标题化合物是一个重要的药物中间体。以2-氨基-5-氯吡啶为起始原料,经溴代和重氮化反应得到目标化合物,总收率为66.31%。其结构经1HNMR、13CNMR和MS确定。该方法具有成本低廉、操作简单且收率较高等优点,符合工业化生产的要求。
关键词:2-碘-3-溴-5-氯吡啶;2-氨基-5-氯吡啶;合成
中图分类号:O626.3 文献标识码:A 文章编号:0258-3283(2017)
Synthesis of 2-Iodo-3-bromo-5-chloropyridine ZHAO Chun-shen*,LI Ting-tao,ZHONG Zhi-xu,LIU Qiang,WANG Ming-yang(College of Pharmacy,Guizhou University,Guiyang 550003,China), Huaxue Shiji, 2017, 39(9)
Abstract:In this work, 2-amino-5-chloropyridine as the starting material, the important intermediate of 2-iodo-3-bromo-5-chloropyridine was prepared by two parts: bromination and diazotization. The structure was confirmed by 1HNMR and MS. The process is low cost, manipulation easily, high yield, and suitable for industrial production. The total product yield was 66.31%.
Key words:2-iodo-3-bromo-5-chloropyridine;2-amino-5-chloropyridine;synthesis
编辑:wq