苯并菲类高分子液晶材料的研究进展
张来齐，孔翔飞*，王桂霞，戴胜平，张洲洋
（桂林理工大学 化学与生物工程学院，广西 桂林 541004）
摘要：苯并菲类衍生物因其优异的柱状相液晶性质和良好的自组装能力，被广泛应用于光电材料，并得到有机合成和光电材料工作者的广泛关注和深入探究。作为苯并菲类衍生物的一个重要分支，高分子液晶材料受到了越来越多的关注。简单介绍了苯并菲类高分子液晶的分类、性质以及各类高分子结构对其液晶性质的影响，对苯并菲类液晶高分子材料的发展历程做简单的综述。
关键词：苯并菲；高分子；光电材料；液晶材料
中图分类号：O61 文献标识码：A 文章编号：0258-3283（2017）
Progressin Triphenylene-based Polymer Liquid Crystal Material ZHANG Lai-qi, KONG Xiang-fei*, WANG Gui-xia, DAI Sheng-ping, ZHANG Zhou-yang (College of Chemistry and Bioengineering, Guilin University of Technology, Guilin 541004,China), Huaxue Shiji, 2017, 39(7)
Abstract: The triphenylene derivatives have been applied in optoelectronic materials due to the excellent columnar liquid crystal properties and well self-assembly. It has been widespread concern and depth study in organic synthesis and optoelectronic materials workers. As an important branch of triphenylene derivatives, the polymer liquid crystal materials have received more and more attentions. In this work, the classifications and properties of triphenylene-based polymer liquid crystal. The influence of the structure of the classifications for its liquid crystal properties were simply introduced and simply review the development of triphenylene liquid crystalline polymer.
Key words: triphenylene; polymer; optoelectronic materials; liquid crystal material
炭基固体碱催化剂的制备和表征及性能研究
朱成龙a，华平*b，喻红梅b，李建华b，朱国华b，王灵光b
（南通大学 a. 纺织服装学院，b. 化学化工学院，江苏 南通 226019）
摘要：分别以葡萄糖、蔗糖、淀粉为载体，KOH为前驱体，采用一步碳化法制得3种固体碱催化剂。通过IR、XRD、SEM和TG-DSC等手段及Hammett指示剂法对催化剂进行了表征，并以三油酸甘油酯与甲醇酯交换反应为探针，比较了三者的催化活性。结果表明，3种催化剂均为无定形碳架结构，较好的热稳定性，在焙烧过程中均有K2CO3晶相生成。催化剂表面碱量与活性呈正相关性，在相同工艺条件下和KOH催化活性相当。
关键词：炭基固体碱；酯交换反应；三油酸甘油酯；甲醇；表征
中图分类号：O643 文献标识码：A 文章编号：0258-3283(2017)
Preparation of Biomass Carbon-based Solid Base Catalyst and Catalytic Activity for Transesterification ZHU Cheng-longa, HUA Ping*b, YU Hong-meib, LI Jian-huab, ZHU Guo-huab, WANG Ling-guangb (a. School of Textile and Clothing, b. School of Chemistry and Chemical Engineering, Nantong University, Nantong 226019 )
Abstract: Three kinds of carbon-based solid base catalysts were prepared by a one-step carbonization method with potassium hydroxide as the precursor and glucose , sucrose,starch as raw materials. The catalysts were characterized by means of IR, XRD, SEM ,TG-DSC and Hammett indicator method. The transesterification of glycerol trioleate and methanol was taken as the probe reaction to compare the catalytic performance for the three kinds of carbon-based solid base catalysts. The results showed that three kinds of carbon-based solid base catalysts were all amorphous carbon structures and had good thermal stability. Potassium carbonate crystalline phase was formed on the carbon-based solid base catalysts during calcination process. The more basicity of the carbon-based solid base catalysts, the better its catalytic activity. It was similar catalytic activity between biomass carbon-based solid base catalysts and potassium hydroxide at the same conditions.
Key words: carbon-based solid base ; transesterification; glycerol trioleate; methanol; characterization
H6P2Mo15W3O62修饰三维金属有机骨架Cu(BDC)(4,4´-Bipy)0.5吸附亚甲基蓝
龚文朋，马海芹，郭改娟，杨水金*
(湖北师范大学化学化工学院污染物分析与资源化技术湖北省重点实验室，湖北黄石 435002)
摘要：采用溶剂热法，在合成金属有机骨架Cu(BDC)(4,4´-Bipy)0.5的过程中引入活性组分H6P2Mo15W3O62，制备出一种新型吸附剂H6P2Mo15W3O62/Cu(BDC)(4,4´-Bipy)0.5。利用IR、XRD、BET、SEM对其结构进行分析，进而研究其亚甲基蓝的吸附性能。研究结果表明，H6P2Mo15W3O62/Cu(BDC)(4,4´-Bipy)0.5对亚甲基蓝有很好的吸附性能，在40℃和pH2的条件下吸附量达78.8 mg/g。H6P2Mo15W3O62/Cu(BDC)(4,4´-Bipy)0.5对亚甲基蓝的吸附符合Langmuir等温吸附型和拟二级动力学方程，吸附过程是一个自发和吸热过程。
关键词：H6P2Mo15W3O62；金属有机骨架；吸附；亚甲基蓝
中图分类号：X703.5 文献标识码：A文章编号：0258-3283（2017）
Adsorption of Methylene Blue by Composites H6P2Mo18O62 Decorating Three-dimensional Framework Cu(BDC)(4,4-Bipy)0.5GONG Wen-peng, MA Hai-qin, GUO Gai-juan, YANG Shui-jin*(College of Chemistry and Chemical Engineering, Hubei Key Laboratory of Pollutant Analysis & Reuse Technology , Hubei Normal University, Huangshi 435002 China)
Abstract：The novel absorbent H6P2Mo15W3O62/Cu(BDC)(4,4-Bipy)0.5 has been prepared by hydrothermal synthesis method, and the active component H6P2Mo15W3O62 was introduced while synthesizing metal organic framework Cu(BDC)(4,4-Bipy)0.5. The structures of the composite were confirmedby IR, XRD, SEM and N2 absorption-desorption experiment, and its MB absorption properties were also investigated. H6P2Mo15W3O62/Cu(BDC)(4,4-Bipy)0.5has great adsorption capacities of the methylene blue. Themaximum adsorption capacity value reached 78.8 mg/g at 40 ℃and pH2. The experiment data could be well described by the Langmuir equations and pseudo-second-order kinetic model. The adsorption process of the composites on methylene blue was spontaneous and endothermic.
Key words：H6P2Mo15W3O62; metal organic frameworks; adsorption; methylene blue
DMDAAC/DMC/IA三元共聚合动力学的研究
宋佳柠，朱明*
（四川师范大学 化学与材料科学学院 四川教育厅特种废水处理工程实验室，四川 成都 610068）
摘要：以二甲基二烯丙基氯化铵（DMDAAC）、甲基丙烯酰氧乙基三甲基氯化铵（DMC）和衣康酸（IA）为共聚合单体，以过硫酸钾-亚硫酸氢钠作氧化还原引发剂，采用膨胀计测定共聚合动力学速率方程和表观活化能，用红外光谱（FT-IR）、热失重分析（TGA）和差示热扫描（DSC）表征两性高分子絮凝剂p(DMDAAC-co-DMC-co-IA)产物。共聚合热力学计算表明，在T<820.5 K实验条件范围内，共聚合自由能变化∆G<0。结果显示，共聚合速率方程为Rp
k[DMDAAC]1.43[DMC]1.36[IA]0.97[引发剂]1.5，表观活化能Ea = 33.3 kJ/mol。
关键词：二甲基二烯丙基氯化铵；甲基丙烯酰氧乙基三甲基氯化铵；衣康酸；聚合动力学
中图分类号：O630 文献标识码：A 文章编号：0258-3283（2017）
Copolymerization Kinetics on DMDAAC/DMC/IA SONG Jia-ning, ZHU Ming* (Sichuan Provincial Key Laboratory of Special Wastewater Treatment, School Chemical and Material Science, Sichuan Normal University, Chengdu 610068,China)
Abstract: The copolymerization kinetics was investigatedby dilatometer method on diallyl dimethyl ammoniumchloride, methacryloxyethyltrimethylammoniumchloride and itaconic acid in aqueous solution using potassium persulfate-sodium bisulfate redox complex initiator. The copolymerization rate equation and apparent activation energy were determined. The copolymerization products p(DMDAAC-co-DMC-co-IA) were confirmed by FT-IR, TGA and DSC. When the temperature was lower than 820.5K, the copolymerization free energy ∆G <0. The polymerization rate equation is Rpk[DMDAAC]1.43[DMC]1.36[IA]0.97[Initiator]1.5, and the activation energy is 33.3 kJ/mol.
Key words: diallyl dimethyl ammoniumchloride; methacryloxyethyltrimethylammoniumchloride; itaconic acid; polymeric kinetic
硝基与杂环取代的N-甲基-4-哌啶酮化合物的合成及活性研究
杨威，刘岩，李宁，刘方正，程浩，王春华，侯桂革*
(滨州医学院 药学院，山东 烟台 264003)
摘要:以芳醛与N-甲基-4-哌啶酮通过Claisen-Schmidt缩合得到两个不对称的N-甲基-4-哌啶酮化合物，并通过NMR、FT-IR、元素分析等进行结构表征。采用MTT法，评价了两种化合物对Hela（宫颈癌细胞）、HePG2（肝癌细胞）、THP-1（人单核巨噬细胞）、SGC-7901（胃癌细胞）的抑制活性以及对LO2（正常肝细胞）的细胞毒性。结果显示，3-(4-吡啶亚甲基)-5-(3-硝基苯亚甲基)-N-甲基-4-哌啶酮显示较好的抑制活性，特别是对THP-1的IC50 = 0.58 µmol/L，而3-(2-噻吩亚甲基)-5-(3-硝基苯亚甲基)-N-甲基-4-哌啶酮的抑制活性稍差，但对正常细胞LO2毒性较小。
关键词: N-甲基-4-哌啶酮；抗肿瘤；细胞毒性；不对称化合物
中图分类号：O657.3 文章标识码:A 文章编号:0258-3283(2017)
Synthesis and Activity of Nitro and Heterocyclic Substituted N-Methyl-4-piperidinone Compounds YANG Wei, LIU yan, LI Ning, LIU Fang-zheng, CHENG Hao, ANG Chun-hua, HOU Gui-ge* (School of Pharmacy, Binzhou Medical University, Yantai 264003，China)
Abstract: Two asymmetricN-methyl-4-piperidinone compounds were synthesized by Claisen-Schmidt condensation reaction of aromatic aldehyde and N-methyl-4-piperidinone. The structures were confirmed by NMR, FT-IR and elemental analysis. Theantitumor activities against Hela, HePG2, THP-1, SGC-7901 and the cytotoxicity for LO2cell lines by MTT method were subsequently evaluated. (3E,5E)-3-(3-nitrobenzylidene)-1-methyl-5-((pyridin-4-yl)methylene)piperidin-4-one shows better inhibitory activity, especially for THP-1 (IC50 = 0.58 μmol/L), while (3E,5E) – 3 -(3-nitrobenzylidene) -1-methyl-5- ((thiophen-2-yl)methylene) piperidin-4-one shows weak inhibitory activity, but the cytotoxicity were markedly lower.
Key words: N-methyl-4-piperidinone; antitumor; cytotoxicity; asymmetric compound
带有12条柔性长链的卟啉及其金属配合物的合成及液晶性质的研究
孙二军*，李艳平，赵仑
(长春师范大学 化学学院，吉林 长春 130032)
摘要：以简单化合物为原料，经过多步反应，合成出一种新型的带有12条肉豆蔻酰氧基取代柔性长链的卟啉配体，并通过与过渡金属盐反应，得到卟啉金属锌、铜配合物。对所合成的化合物通过红外光谱、紫外-可见吸收光谱、1HNMR等进行表征。通过荧光发射光谱、荧光寿命等进行了光学性质研究；并通过差示扫描量热法和偏光显微镜研究了化合物的液晶性质。结果表明，卟啉配体与铜配合物是双变液晶，而锌配合物在升温时呈现液晶相。化合物液晶相的相变温度较低，相变区间较窄。
关键词：卟啉；肉豆蔻酰氧基；合成；液晶
中图分类号: O 621.3 文献标识码: A 文章编号：0258-3283（2017）
Synthesis and Liquid Crystalline Property of 5, 10, 15, 20-Tetra (3, 4, 5-trimyristoyloxyphenyl) porphyrin and Its Metal Complexes SUN Er-jun*, LI Yan-ping, ZHAO Lun (College of Chemistry, Changchun Normal University, Changchun, 130032, China)
Abstract: After a series of reaction, a new porphyrin ligand and its transition metal zinc and copper complexes with 12 myristoyloxy substituted long flexible chains were synthesized and confirmedby UV-vis spectra, infrared spectra, and 1HNMR spectra. The liquid-crystalline behaviors of these compounds were also investigated by differential scanning(DSC) and polarizing optical microscopy (POM). Research showed that porphyrin ligand and copper complex are dual variable liquid crystals, while zinc porphyrin complex shows liquid crystalline phase when heated. The phase transition temperatures of these compounds are low and the temperature ranges of liquid crystal are narrow.
Key words: porphyrin; myristoyloxy; synthesis; liquid crystal
LSD1小分子抑制剂的合成及抗肿瘤活性研究
周鑫鑫*，周宁，刘长春
(江苏食品药品职业技术学院 药学院，江苏 淮安 223003)
摘要：设计并合成了一系列以苯甲酰肼类结构为母核的赖氨酸特异去甲基化酶1(LSD1)小分子抑制剂，并研究其体外抗肿瘤活性。首先，通过体外酶水平单浓度抑制实验进行了初步评价，并随后进一步考察目标化合物对多种LSD1高表达肿瘤细胞株增殖的抑制作用，化合物经质谱及核磁共振表征确证。活性评价实验结果显示，3-(((3R，5S)-3, 5-二甲基吗啉代)磺酰基)-N'-(7-羟基-2, 3-二氢-1H-茚-1-亚基)苯甲酰肼、N'-(1-(5-氯-2-羟基苯基)亚乙基)-3-(((3R，5S)-3, 5-二甲基吗啉代)磺酰基)苯甲酰肼和N'-(4-氯-7-羟基-2, 3-二氢-1H-茚-1-亚基)-3-((4-吗啉代哌啶-1-基)磺酰基)苯甲酰肼可显著抑制肿瘤细胞的增殖，并有4个目标化合物对体外多种LSD1高表达的肿瘤细胞株增殖有抑制作用，其中3-(((3R，5S)-3, 5-二甲基吗啉代)磺酰基)-N'-(7-羟基-2, 3-二氢-1H-茚-1-亚基)苯甲酰肼对BGC823、HCT116、A2780s的半数抑制浓度分别为0.32、0.54、0.90 μmol/L。
关键词：LSD1；小分子抑制剂；合成；抗肿瘤活性
中图分类号：R914.5 文献标识码：A 文章编号：0258-3283（2017）
Synthesis and Anti-tumor Activity of Small Molecule Inhibitors of LSD1 ZHOU Xin-xin*, ZHOU Ning, LIU Chang-chun (School of Pharmacy, JiangSu Food & Pharmaceutical Science College, Huaian 223003, China)
Abstract：A series of small molecule inhibitors of LSD1 were synthesized based on the structure of benzoyl hydrazine, and the anti-tumor activities in vitro were investigated. By the compound obtained in vitro enzyme inhibition level single concentration, and the anti-proliferative activity of the compounds for a variety of LSD1 tumor cell lines has been tested. The chemical structure of target compound were confirmed by ESI-MS and NMR. MTT assay showed that compound 3-((3R,5S)-3,5-dimethylmorpholinosulfonyl)-N'-(7-hydroxy-2,3-dihydroinden-1-ylidene)benzohydrazide, N'-(1-(5-chloro-2-hydroxyphenyl)ethylidene)-3-((3R,5S)-3,5-dimethylmorpholinosulfonyl)benzohydrazide and N'-(4-chloro-7-hydroxy-2,3-dihydroinden-1-ylidene)-3-(4-morpholinopiperidin-1-ylsulfonyl)benzohydrazide significantly inhibited tumor cell proliferation. Four target compounds showed inhibitory effect on the proliferation of tumor cell lines with high expression of LSD1 in vitro. The half of the compound3-((3R,5S)-3,5-dimethylmorpholinosulfonyl)-N'-(7-hydroxy-2,3-dihydroinden-1-ylidene)benzohydrazide for BGC823, HCT116, A2780s inhibitory concentration (IC50) was 0.32, 0.54, 0.90 μmol/L.
Key words：lysine-specific demethy-lase l (LSD1); small molecule inhibitors; synthesis; anti-tumor activity
三乙胺三氟化氢在含氟脂肪族化合物合成中的应用
马辉*，王博，谷玉杰，王伟，吕剑
（西安近代化学研究所，陕西西安 710065）
摘要：三乙胺三氟化氢作为一种向化合物分子中引入氟原子的有效氟化试剂，具有较小的腐蚀性、温和的反应活性以及良好的区域选择性，在含氟化合物的合成中有着广泛的应用。综述了三乙胺三氟化氢在含氟脂肪族化合物合成中的应用，重点介绍采用亲核氟化、亲电氟化、环氧开环氟化和电化学氟化进行的反应。
关键词：三乙胺三氟化氢；含氟脂肪族化合物；氟化反应；应用
中图分类号:O623 文献标识码:A 文章编号：0258-3283（2017）
Application of TriethylamineTris(hydrofluoride)on the Synthesis of Fluorinated Aliphatic CompoundsMA Hui*, WANG Bo, GU Yu-jie, WANG Wei, LV Jian(Xi'an Modern Chemistry Research Institute, Xi'an 710065, China)
Abstract:As an effective fluorinating reagent for introducing fluorine atoms into organic molecules, triethylaminetris(hydrofluoride) is widely used in the synthesis of fluorinated compounds because of its low corrosivity, mild reaction activity and good region selectivity. In this work, several applications of triethylaminetris(hydrofluoride) on the synthesis of fluorinated aliphatic compounds are reviewed based on the type of reaction，especially for nucleophilic fluorination, electrophilic fluorination, ring-opening fluorination of epoxide and electrochemical fluorination.
Keywords：triethylaminetris(hydrofluoride); fluorinated aliphatic compounds; fluorination reaction; application
新型抗精神病药物盐酸鲁拉西酮的合成研究进展
祁秀秀*，陈文华，郭亚楠
（常州工程职业技术学院 制药与环境工程系，江苏 常州 213164）
摘要：盐酸鲁拉西酮是一种新型的抗精神病药物。本文归纳了该原料药的合成方法，根据起始原料的光学纯度、中间体的不同可将合成路线分为三大类，并且对这三类方法进行了比较分析，总结出各自的优缺点，从而为该原料药的制备研究提供参考。
关键词：盐酸鲁拉西酮；抗精神病；合成
中图分类号: O629.7 文献标识码: A
SynthesisProgress of New Atypical AntipsychoticLurasidone Hydrochloride QI Xiu-xiu*, CHEN Wen-hua, GUO Ya-nan (Department of Pharmaceutical and Environmental Engineering, Changzhou Vocational Institute of Engineering, Changzhou 213164)
Abstract: Lurasidone hydrochloride is a new atypical antipsychotic. In this work, synthetic methods of the medicine were summarized. These methods were categorized into three classes based on the optical purity of starting materials and intermediates involved. Also, the merits and disadvantages of these synthetic routes were discussed, and reference for preparation of the medicine was provided.
石墨烯修饰电极差分脉冲伏安法测定溴氰菊酯的研究
王俊博，董泽刚，兰天宇, 王贵，杜海军*
(贵州民族大学 化学与生态环境工程学院，贵州 贵阳 550025)
摘要：运用循环伏安法、差分脉冲伏安法等测试技术研究了溴氰菊酯在石墨烯修饰电极上的电化学行为，建立了一种间接测定溴氰菊酯的电化学分析方法。结果表明，与玻碳电极相比，石墨烯修饰电极能显著提高溴氰菊酯水解产物的还原峰电流。在优化的实验条件下，溴氰菊酯水解产物的还原峰电流与溴氰菊酯浓度在1.0×10-6 ～ 1.0×10-4 mol/L范围内呈较好的线性关系，最低检出限为5.7×10-7 mol/L。该石墨烯修饰玻碳电极具有较好的重现性，用于测定陈皮中的溴氰菊酯，效果良好。
关键词：溴氰菊酯；石墨烯；差分脉冲伏安法
中图分类号：O657.1 文献标识码：A 文章编号：0258-3283（2017）
Determination of Deltamethrin by Differential Pulse Voltammetry with Graphene Modified Glassy Carbon Electrode WANG Jun-bo, DONG Ze-gang, LAN Tian-yu, WANG Gui, DU Hai-jun*(College of Chemistry and Eco-Environmental Engineering, Guizhou Minzu University, Guiyang 550025 )
Abstract: The electrochemical behavior of deltamethrin at the graphene modified glassy carbon electrode (Gr/GCE) was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The experimental parameters were optimized, and a electroanalytical method for determining deltamethrin was developed. The reduction peak current of the hydrolysis product of deltamethrin was enhanced significantly at the Gr/GCE, in contrast to that obtained at the bare GCE. Under the optimized experimental conditions, the reduction peak current was proportional to the deltamethrin concentration in the ranges of 1×10-6 ～ 1×10-4 mol/L with a detection limit of 5.7×10-7 mol/L. The graphene nanosheets modified glassy carbon electrode is easy to be prepared with good reproducibility. The proposed methodology was successfully applied to the detection of deltamethrin in the dried orange peel with satisfactory results.
Key words: deltamethrin; graphene; differential pulse voltammetry
ICP-OES和ICP-MS测定天然棕色棉和染色棕棉中24种元素含量
王晓娟*1,2，桂家祥3，杨力生1,2，林振兴1,2
（1. 宁波出入境检验检疫局，浙江 宁波 315012；2. 宁波检验检疫科学技术研究院，浙江 宁波 315012；3. 赣州出入境检验检疫局，江西 赣州 332000）
摘要：采用微波消解对天然棕色棉和染色棕棉样品进行处理，通过电感耦合等离子体发射光谱法和电感耦合等离子体质谱法测定其中B、Na、Mg、Al、P、K、Ca、Ti、V、Mn、Fe、Co、Ni、Cu、Zn、Ga、Se、Rb、Sr、Mo、Ag、Cs、Ba、U等24种元素的含量。结果表明，与染色棕棉相比，天然棕色棉中B、Mg、P、K、Ca、Ti、V、Mn、Rb、Mo等元素含量显著偏高（P＜0.05），Na元素含量显著偏低（P＜0.05），采用聚类分析（最短距离法）对样品中24种元素含量进行处理，可正确判断天然棕色棉和染色棉。
关键词：天然棕色棉；电感耦合等离子体发射光谱；电感耦合等离子体质谱；无机元素；聚类分析
中图分类号：O657.3 文献标识码：A 文章编号：0258-3283（2017）
Determination of 24 Elements in Naturally Brown Cotton and Dyed Brown Cotton by ICP-OES and ICP-MS WANG Xiao-juan*1,2, GUI Jia-xiang3, YANG Li-sheng1,2, LIN Zhen-xing1,2(1. Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012; 2. Ningbo Academy of Inspection and Quarantine, Ningbo 315012; 3. Ganzhou Entry-Exit Inspection and Quarantine Bureau, Ganzhou 332000)
Abstract: The content of B, Na, Mg, Al, P, K, Ca, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, Ga, Se, Rb, Sr, Mo, Ag, Cs, Ba, U in naturally brown cotton and dyed brown cotton were determined by the means of ICP-OES and ICP-MS coupled with microwave digestion. Compared with those in the dyed cotton, the content of B, Mg, P, K, Ca, Ti, V, Mn, Rb, Mo in naturally brown cotton samples were significant higher (P<0.05), while the content of Na in naturally brown cotton samples was much lower (P<0.05). The single linkage method of cluster analysis was applied to evaluate 24 elements in all the samples, which exhibited the ability to effectively differentiate the naturally brown cotton samples from dyed colored samples.
Key words: naturally brown cotton; ICP-OES; ICP-MS; inorganic element; cluster analysis
高效液相色谱法测定白蚁防治药土屏障中的吡虫啉和伊维菌素
宋玉梅，何建强*，刘杰恒，马艳芳
（中国广州分析测试中心 广东省测试技术公共实验室
广东省化学危害应急检测技术重点实验室，广东 广州 510070）
摘要：建立了测定白蚁防治药土屏障中的吡虫啉和伊维菌素的高效液相方法。目标物经甲醇提取后，经SPE小柱净化，超高效液相色谱分离测定，分别进行了两个添加水平的加标回收实验。吡虫啉平均回收率：粘土96.05 % ～ 99.28 %，RSD为2.60 %～3.26 %；砂土82.16 %～83.55 %，RSD为2.00%～2.28%。伊维菌素平均回收率：粘土93.00 %～110.56 %，RSD为 2.31 %～4.69 %；砂土101.63 % ～ 101.70 %，RSD为2.59 %～5.12 %。方法简单，灵敏度高，重现性好。
关键词：高效液相色谱;吡虫啉;伊维菌素;白蚁防治
中图分类号：O652.1 文献标识码：A 文章编号：0258-3283（201*）
Determination of imidacloprid and ivermectin in chemical soil barrier by HPLC Song Yu-Mei, He Jiang-Qiang*, Liu Jie-Heng, MA Yan-fang (Guangdong Provincial Public Laboratory of Analysis Testing Technology，Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals，China National Analytical Center ( Guangzhou) ，Guangzhou 510070，China)
Abstract: To develop methods for Determination of imidacloprid and ivermectin in chemical soil barrier by HPLC. By extraction with methanol, futher cleanup was performed on ENVI-18 SPE column. The connent of imidacloprid and ivermectin were determined by HPLC. Tests for recovery were made by addition of two target compounds at two different concentration levels to two kinds of soils. The mean recoveries of imidacloprid and ivermectin in clay soil ranged from 96.05 % to 99.28 % and 93.00 % to 110.56 %, and RSD were 2.60 % to 3.26 % (n = 6), and2.31 % to 4.69 % (n = 6),respectively. The mean recoveries of imidacloprid and ivermectin in sand soil ranged from 82.16 % to 83.55 % and 101.63 % to 101.70 % , and RSD were 2.00% to 2.28% (n = 6), and 2.59 % to 5.12 % (n = 6), respectively. The methods are simple, high sensitivity and good reproducibility.
Key words: HPLC; imidacloprid ; ivermectin ; termite prevention
测定尿液中血红蛋白含量的共振散射新方法
唐宁莉*，单展，范晶晶，吴美茜
（桂林理工大学 化学与生物工程学院，广西 桂林 541004）
摘要：在酸性介质中，锌试剂和血红蛋白通过静电引力作用生成离子缔合物，导致体系的共振散射信号增强，据此建立了一种简单、灵敏、快速测定血红蛋白含量的共振散射光谱新方法。在优化的实验条件下，λ = 605 nm处，血红蛋白浓度在0.04 ～ 1.20 μg/mL范围内与体系共振散射强度的增加值（△I）呈良好的线性关系，线性回归方程△I = 113.43ρ － 0.5170(μg/mL)，相关系数r = 0.9983，方法检出限为0.02 μg/mL。将该方法应用于尿样中血红蛋白含量的检测，回收率为93.40% ～ 106.66%，结果令人满意。
关键词：锌试剂；血红蛋白；尿液；共振散射
中图分类号：O657. 3 文献标识码：A 文章编号：0258-3283（2017）
A New Resonance Light Scattering Method for the Determination of Hemoglobin in the Urine TANG Ning-li *, SHAN Zhan, FAN Jing-jing, WU Mei-xi (College of Chemistry and Biological Engineering, Guilin University of Technology, Guilin 541004, China)
Abstract: Zinconreacted with hemoglobin to form ion-association complexes through electrostatic effects in acidic medium, which greatly enhanced the resonance light scattering intensity. So a simple, sensitive and rapid method for the determination of trace amounts of hemoglobin was established. Under the optimal conditions,the increased intensity(ΔI) was linear to the concentration of hemoglobin in the range of 0.04 ～ 1.20 μg/mL at the wavelength of 605 nm, equation of linear regression △I = 113.43ρ - 0.5170, with a correlation coefficient of 0.9983 and a detection limit of 0.02 μg/mL.This method has been applied to the determination of hemoglobin in the urine samples with satisfactory results, the recoveries were in the range of 93.40% ～ 106.66%.
Key words: zincon; hemoglobin; urine samples; resonance light scattering
基于国家标准物质资源共享平台探讨我国标准物质
发展现状与趋势
（中国兵器工业集团第五三研究所，山东 济南 250031）
摘要：标准物质是我国计量法中依法管理的计量标准，是开展化学、生物、工程与物理量有效测量所必须的标尺和砝码。通过国家标准物质资源共享平台收录的标准物质信息对我国各应用领域中标准物质的发展现状与趋势进行了介绍，对主要标准物质研制单位情况进行了介绍。
关键词：标准物质；国家标准物质资源共享平台；现状；趋势
中图分类号：O652.3 文献标识码：A 文章编号：
Status and Tendency of Reference Materials Based on National Sharing Platform for Reference Materials Resource ZHAO Hui*, ZHAO Hua, LIU Yuan-dong, HUANG Hui，LI Ying, GONG Chen (China North Industries Group Corporation Institute 53, Jinan 250031)
Abstract: The reference material is the standard of measurement in metrology law of China, it is necessary to carry out the effective measurement of chemical, biological, engineering and physical quantities. This work introduces the development status and tendency of reference material in variousfields and the main development status of reference material producers of China based on National Sharing Platform for Reference Materials Resource.
Key words: reference material; national sharing platform for reference materials resource; status; tendency
一种新型罗丹明类双通道荧光探针
及其对Fe3+和Cu2+的选择性识别研究
沈文通1，成春文2, 3，王风贺*2，雷武3，夏明珠3，王风云3
（1. 江苏省阜宁县危险化学品管理办公室，江苏 盐城 224400；2. 南京师范大学 环境学院 江苏省物质循环与污染控制重点实验室，江苏 南京 210023；3. 南京理工大学 工业化学研究所，江苏 南京 210094 ）
摘要：以罗丹明B、水合肼和吡啶-2-甲醛为反应物，合成了一种新型的罗丹明类Fe3+和Cu2+双通道分子探针(Fluorescent probe，FP)，并用核磁和质谱对其分子结构进行了表征。利用荧光分光光度计和紫外可见分光光度计研究了FP对Fe3+、Cu2+等14种金属离子的识别性能。研究结果表明，在V（CH3OH）︰V（H2O）= 1︰1体系中，当选用荧光光谱分析时，探针FP对Fe3+具有良好的选择性响应，且Fe3+在2 ~ 30 μmol/L时，探针荧光强度与Fe3+浓度呈线性关系，线性相关系数为0.998。而当选用紫外可见光谱分析时，探针FP对Cu2+具有很好的选择性响应，且当Cu2+浓度为0 ~ 9 μmol/L时，探针FP的吸光度与Cu2+浓度呈线性关系，线性相关系数为0.999。
关键词：荧光探针；罗丹明B；识别；Cu2+；Fe3+
中图分类号: O657.3 文献标识码: A 文章编号: 0258-3283（2017）
Synthesis of New Dual Fluorescent Probe Based on Rhodamineand Performance in Selective Recognition of Fe3+ and Cu2+ SHEN Wen-tong1, CHENG Chun-wen2,3, WANG Feng-he*2, LEI Wu3, XIA Ming-zhu3, WANG Feng-yun3 (1.Office of Hazardous Chemicals Management in Funing County, Yancheng 224400 China; 2. Jiangsu Provincial Key Laboratory of Materials Cycling and Pollution Control, School of Environment, Nanjing Normal University, Nanjing 210042; 3. Industrial Chemical Institute, Nanjing University of Science and Technology, Nanjing 210094, China)
Abstract: A novel Rhodamine-based dual fluorescent probe (FP) for detecting Fe3+ and Cu2+ was designed and synthesizedusing rhodamine B, hydrazinehydrate, and pyridine- formaldehyde as raw reactants. Themolecule structure of FP was confirmedby 1H NMR and MS, and theselective recognition properties in detecting Fe3+, Cu2+, and other 12 different kinds of metal ionswere investigated by fluorescent spectroscopy and UV-Vis spectroscopy. The results revealed that FP had a high selectivity and sensitivity for Fe3+ using fluorescence spectra, and for Cu2+ via UV-vis absorption spectra in CH3OH-H2O (1/1, V/V). When the concentration of Fe3+ and Cu2+ was respectively in 2-30 μM and 0-9 μM, there was a good linearity relationship between the targeted metal ion of Fe3+ and Cu2+ and their fluorescence intensity and UV-vis absorption, and thecoefficient values were more than 0.999.
Key words: fluorescent probe; Rhodamine B; recognition; Cu2+; Fe3+
一种用于废水中重金属吸附的磁性纳米材料制备
吴孝兰*1，肖瑞丽2，赵雅梦2，凌芳1，刘征宙1
（1. 国药集团化学试剂有限公司，上海 200002；
2. 华东理工大学 化学与分子工程学院，上海 200237）
摘要：水体中大量的重金属离子严重威胁着水生物和人类的生存健康。磁性纳米材料特有的表面效应和磁响应特性，使其在作为重金属离子吸附剂时具有高效回收、脱附简单、避免对水体的二次污染等优点。本文制备了一种用于吸附废水中重金属的磁性纳米材料，以戊二醛（GA）为间隔臂，将聚乙烯亚胺（PEI）修饰在商品化的四氧化三铁磁球上。最终得到一种用于富集废水中重金属的磁性纳米材料Fe3O4@SiO2@GA@PEI。
关键词：纳米材料；重金属；富集
中图分类号：O614.811 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of Magnetic Nanoparticles for the Enrichment of Heavy Ions in Waste Water WU Xiao-lan*1, XIAO Rui-Li 2，ZHAO Ya-meng2，LING Fang 1，LIU Zheng-zhou1 (1. Sinopharm Chemical Reagent Co., Ltd, Shanghai 200002, China; 2. College of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China), Huaxue Shiji, 2017, 39(7)
Abstract: Heavy ions in the water threaten the survival of aquatic organisms and human health seriously. Magnetic nanoparticles have the special surface effect and magnetic response characteristics, which have advantages in the enrichment of heavy ions such as high efficiency recovery, simple desorption, avoid secondary pollution of water body. In this work, a magnetic nanoparticles for the adsorption of heavy metals in wastewater was prepared using Glutaraldehyde (GA) as spacer arm. Polyethyleneimine (PEI) was modified on commercial Fe3O4. Finally, a facile nanomaterial Fe3O4@SiO2@GA@PEI was prepared for the enrichment of heavy ions.
Key words: nanomaterials; heavy ions; enrichment
一种新型咔唑席夫碱的合成及对Fe3+荧光识别研究
周钰莹a，吕永军*a,b
(四川理工学院 a. 化学工程学院，b. 材料腐蚀与防护四川省重点实验室，四川 自贡 643000)
摘要：以9-氨基咔唑与2-羟基-1-萘甲醛为原料，设计合成了一种新型咔唑类席夫碱化合物。通过核磁共振光谱、质谱、红外光谱和元素分析对其结构进行表征，利用荧光光谱研究了目标化合物对不同金属离子的荧光识别性能，采用质谱和密度泛函理论（DFT）分析其与Fe3+结合作用模式。结果表明，目标化合物通过荧光猝灭可选择性识别Fe3+，原因是与Fe3+配位后引发了分子内的光诱导电子转移过程。
关键词：咔唑；席夫碱；荧光识别；Fe3+
中图分类号：O657.3 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of Novel Carbazole-based Schiff Base and Fe3+ Fluorescence Spectral Recognition ZHOU Yu-yinga, LV Yong-jun*a, b (a. College of Chemical Engineering, b. Material Corrosion and Protection Key Laboratories of Sichuan Province, Sichuan University of Science and Engineering, Zigong 643000, China), Huaxue Shiji, 2017, 39(7)
Abstract: A novel carbazole-based Schiff base compound was synthesized from 9-amino-carbazole and 2-hydroxy-1-naphthaldehyde. The structure was confirmed by 1HNMR, ESI-MS, IR and elemental analyses. Cation sensing properties were investigated by fluorescence spectra. Proposed binding mode and Fe3+ was revealed by ESI-MS and density functional theory (DFT) method. The results indicated that the compound could selectively sense Fe3+ by fluorescence quenching, which can be ascribed to the initiation of photo induced electron transfer process afterward Fe3+ coordination.
Key words：carbazole；Schiff base；fluorescence sensing；Fe3+
有效的[4+1]/[3+2+1]双环化反应构建茚并氧杂蒽杂环骨架及其晶体结构
高侠1，朱晓彤*2, 3
(1. 江苏省徐州医药高等职业学校，江苏 徐州 221116; 2. 徐州医科大学公共教育学院，江苏 徐州 221004; 3. 中国矿业大学化学化工学院，江苏 徐州 221116)
摘要：茚并氧杂蒽类化合物C24H28O5是由邻苯二甲醛和5, 5-二甲基-1, 3-环己二酮在醋酸溶剂中，经室温下搅拌一步法反应制得。结构通过单晶X-射线衍射法测定，其晶体属单斜晶系，空间群P2(1)，晶胞参数a = 1.00692(11) nm，b = 1.02173(12) nm，c = 2.4306(2) nm，V = 2.5006(5) nm3，Z = 4，晶胞密度Dc = 1.247 mg/ m3，吸收系数μ = 0.087 mm-1，单胞中电子的数目F(000) = 1008，分子量Mr = 469.56(单晶中包含一分子溶剂DMF)。晶体结构经全矩阵最小二乘法对各原子参数进行修正，最终得到的偏离因子为R = 0.0619，ωR = 0.0904。在晶体结构中新形成的茚环呈现信封式构象，同时形成的吡喃环显示为扭船式构象。
关键词: 简便合成；室温；一步法；晶体结构
中图分类号：O626 文献标识码：A 文章编号：0258-3283（2017）
Effective Indeno Xanthene Heterocycle Compound and Crystal Structure Based on [4+1]/[3+2+1] Dicyclic Reaction Gao Xia1, ZHU Xiao-Tong*2,3 (1. Jiangsu Provincial Xuzhou Pharmaceutical Vocational College, Xuzhou 221116, China; 2. School of Basic Education Sciences, Xuzhou Medical University, Xuzhou 221004, China; 3. School of Chemical Engineering & Technology, China University of Mining and Technology, Xuzhou 221116, China)
Abstract: The indeno xanthene heterocycle compound C24H28O5 has been one-step synthesized by the reaction of o-phthalaldehyde and 5,5-dimethyl-1,3-cyclohexanedionein acetic acid by stirring at room temperature. The structure was determined by single crystal X-ray diffraction. The crystal is monoclinic, space group P2(1), with Mr = 469.56( A molecular solvent of DMF was included in the crystal), a = 1.00692(11) nm, b = 1.02173(12) nm, c = 2.4306(2) nm, V = 2.5006(5) nm3, Z = 4, Dc = 1.247 mg/m3, μ = 0.087 mm- 1, F(000) = 1008. The structure was solved by direct methods and refined by full-matrix least squares method to the final R = 0.0619，ωR= 0.094. X-ray analysis reveals that the newly formed pyran-ring in the crystal structure is the skew boat conformation, while the indene ring is the envelope conformation.
Key words: simple synthesis; room temperature; one-step; crystal structure
阿维巴坦钠工艺杂质的合成研究
钟霞，陈年根*
（海南医学院药学院，海南 海口 571199）
摘要：研究了阿维巴坦钠工艺杂质的合成工艺，以便对阿维巴坦钠的质量进行控制。以(2S, 5R)-5-[(苄基氧基)氨基]哌啶-2-甲酸乙酯草酸盐为起始原料，经缩合、水解、磺酰胺化、脱保护、磺酰化、盐交换等反应制备(2S, 5R)-7-氧代-N-磺酸基-6-磺酸氧基-1,6-二氮杂双环[3.2.1]辛烷-2-甲酰胺二钠盐。目标产物的化学结构经质谱、1HNMR和13CNMR等确证，纯度为99.3%，总收率为15.7%(以原料计算)。该工艺反应条件温和、操作简便，为阿维巴坦钠工艺杂质的合成提供了一种新选择。
关键词：阿维巴坦钠；β-内酰胺酶抑制剂；工艺杂质
中图分类号：0643.3 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of Impurity inAvibactam Sodium ZHONG Xia, CHEN Nian-gen*( College of Pharmacy, Hainan Medical University, Haikou 571199, China )
Abstract: To conduct the quality control of avibactam sodium, the impurity (2S, 5R)-7-oxo-N-sulfo-6-sulfooxy-1,6-diazabicyclo[3.2.1]octane-2-carboxamidedisodium salt generated in the synthetic process of avibactam sodium wassynthesized. The impurity was synthesized from(2S,5R)-ethyl 5-(benzyloxyamino)piperidine-2-carboxylate oxalate as raw material viacondensation, hydrolysis, sulfonamidation, deprotection of benzyl group, sulfonylation and base replacement. The results showed that the purity was 99.3%, and the total yield was 15.7%. The chemical structurewasconfirmed by MS, 1 HNMR and 13CNMR. The process was simple and a new choice for production of the process impurity inavibactam sodium.
Key words: Avibactam sodium; β-Lactamaseinhibitors; process impurity
五氟磺草胺中间体2-丙硫基-3-三氟甲基苯酚合成工艺改进
陈明珠，辜顺林，严生虎，刘建武，张跃*
（常州大学 流动化学与过程工程研究所，江苏 常州 203164）
摘要：提出了一种制备五氟磺草胺中间体2-丙硫基-3-三氟甲基苯酚的改进工艺。以间三氟甲基苯酚为原料，安全无毒的3, 4-2H-二氢吡喃替代剧毒品氯甲基甲醚作为酚羟基保护剂，保护后的产物经硫醚化、水解反应，“一锅法”得到标题化合物，总收率达74.6%，产物纯度达99.5%。
关键词：五氟磺草胺；2-丙硫基-3-三氟甲基苯酚；工艺改进
中图分类号：TQ031.2 文献标识码：A 文章编号：0258-3283（2017）
Improved Process of 2-Propylthio-3-trifluoromethyl-phenol as Intermediate of Penoxsulam CHEN Ming-zhu, GU Shun-lin, YAN Sheng-hu, LIU Jian-wu, ZHANG Yue*（Institute of Flow Chemistry & Process Engineering, Changzhou University, Changzhou 213164, China）, Huaxue Shiji, 2017, 39(8)
Abstract: An improved process was proposed to synthesize 2-propyl-3-trifluoromethylphenol, a key intermediate of penoxsulam, in a total yield of 74.6% with 99.5% product purity. The new route employed m-trifluoromethylphenol as raw material and 3, 4-dihydro-2H-pyran as phenolic hydroxylprotective agent. The target product was obtained by thioetherification and hydrolysis sequentiallyin a one-pot way. Comparing with hypertoxic traditional agent such as hypertoxicchloromethyl methyl ether, 3, 4-dihydro-2H-pyran safer and fairly low toxicity.
Key words: penoxsulam; 2-propyl-3-trifluoromethylphenol; improved process
一锅法制备四氢苯并呋喃衍生物
黄瑶，胡若飞*，邹发凯，吴丽惠，石文业，和平*
（湖北文理学院 化学工程与食品科学学院，湖北 襄阳 441053）
摘要：以取代苯乙酮为起始原料，经由分子碘的卤代，与吡啶成盐得到氮叶里德化合物，再进一步在碱存在下与1，3-环己二酮、取代苯甲醛反应，一锅法高收率制备得到标题化合物，该方法不需提前制备a-卤代苯乙酮或者不饱和羰基化合物，具有操作简便、条件温和、收率较高等特点。目标产物经过了1HNMR、13CNMR、IR和MS确认表征。
关键词：一锅法反应；合成；四氢苯并呋喃；苯乙酮
中图分类号：o626.11 文献标识码：A 文章编号：0258-8283（2017）
One-pot Synthesis of Tetrahydrobenzofuran Derivatives HUANG Yao, HU Ruo-fei*, ZOU Fa-kai, WU Li-hui, SHI Wen-ye, HE Ping* (College of Chemical Engineering and Food Science, Hubei University of Arts and Science, Xiangyang 441053, China), Huaxue Shiji, 2017, 39(8)
Abstract: A general one-pot synthesis of tetrahydrobenzofurans was developed, which starting from substituted acetophenones, benzaldehydes, and 1,3-cyclohexanedione, the key point of this method is the formation of the ylide in one pot just by halogenation of the acetophenone with the assistance of pyridine. This approach has many advantages over conventional ones, such as mild reaction conditions, simple experimental procedures and high yields, as well as without needing to synthesis of a-haloacetophenone or unsaturated carbonyl compound in advance. And all the target product was confirmed by 1HNMR, 13CNMR, IR and MS.
Key words：one-pot reaction；synthesis；tetrahydrobenzofuran；acetophenone
4-氟-1-萘酚的合成
赵春深*a, b，凌志新b，闫沛沛b，黄筑艳a
(贵州大学a.药学院，b.化学与化工学院贵州省发酵工程与生物制药重点实验室，贵州贵阳550003)
摘要：以1-氟萘为起始原料，经卤代、硼酸基团取代卤素以及硼酸基水解3步反应合成重要的医药化工中间体，即标题化合物。该合成方法未见文献报道，原料易得，成本低廉且收率较高。
关键词：1-氟萘；4-氟-1-萘酚；合成
中图分类号：O626.3 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of 4-Fluoro-1-naphthalenol ZHAO Chun-shen*a,b, LING Zhi-xinb, YAN Pei-peib, HUANG Zhu-yana(a.School of Pharmaceutical Sciences; b.School of Chemistry and Chemical Engineering, Key Laboratory of Guizhou for Fermentation Engineering and Biomedicine, Guizhou University, Gui yang 550003）
Abstract: 1-Fluoronaphthaleneas a starting material, the important intermediate of 4-fluoro-1-naphthalenol was synthesizedvia three steps: halogen substituted, boric acid group substituted halogen and the hydrolysis ofboric acid group.Noreports on the synthesis ofthis compoundwas foundin the literature, and the synthesisisraw materials easy to be found,low cost,the high total yield.
Keywords：1-fluoronaphthalene; 4-fluoro-1-naphthalenol; synthesis
沙格列汀的合成
王建塔a, b，杨果a，蔡进a，张毅a, b，汤磊*a, b
（贵州医科大学 a. 药学院，b. 贵州省化学合成药物研发利用工程技术研究中心，贵州 贵阳 550004）
摘要：以金刚烷乙酸为起始原料，经溴代、混酸氧化、氨解、氨基Boc保护以及(1R, 2S)-2-氨基-1, 2-二苯基乙醇拆分得到(S)-N-叔丁氧羰基-3-羟基-1-金刚烷甘氨酸，之后再与(1S, 3S, 5S)-2-氮杂二环[3.1.0]己烷-3-甲酰胺对甲苯磺酸盐在HATU条件下缩合得到N-[(1S)-2-[(1S, 3S, 5S)-3-氨甲酰基-2-氮杂双环[3.1.0]己烷-2-基]-1-(3-羟基-1-金刚烷)-2-氧代乙基]氨基甲酸叔丁酯，最后经酰胺脱水、氨基脱保护反应得到沙格列汀，总收率为16.1%，纯度为99.8%，e.e.＞99.9%。
关键词：沙格列汀；2型糖尿病；合成
中图分类号：R914 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of Saxagliptin WANG Jian-ta a,b, YANG Guoa, CAI Jina, ZHANG Yi a,b, TANG Lei*a,b（a. School of Pharmacy, b. Guizhou Chemical Drug Research and Development Engineering Technical Center, Guizhou Medical University, Guiyang 550004, China）
Abstract: The key intermediate(S)-N-Boc-3-hydroxyadamantylglycine was synthesized from 1-adamantaneacetic viabromination,oxidation, ammonolysis, amino protection and resolution, which was condensed with (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamide p-toluenesulfonate to give tert-Butyl [(1S)-2-((1S,3S,5S)-3-carbamoyl-2-azabicyclo[3.1.0]hexan-2-yl)-1-(3-hydroxytricyclo[3.3.1.13,7]decan-1-yl)-2-oxoethyl]carbamate, and then followed by dehydration and deprotection to afford the title compound saxagliptin with an overall yield of 16.1% , purity 99.8%, e.e.＞99.9%.
Key words:saxagliptin; type 2 diabetes mellitus; synthesis
3,4-二甲基苯胺的合成研究
崔凯1，沈宏*2
（1．南京大学金陵学院 化学与生命科学学院，江苏 南京 210089；
2．江苏开放大学，江苏 南京 210036）
摘要：分别以邻二甲苯和对硝基甲苯为起始原料，通过两种不同方法制备标题化合物。邻二甲苯经酰化、成肟、贝克曼重排、水解得到目标产物，纯度达99%，总收率53%。以对硝基甲苯为原料，经N-（2-甲基-5-硝基苄基）乙酰胺中间体合成标题化合物，纯度达99%，总收率50%。产物均经红外、核磁、质谱确认结构。
关键词：3,4-二甲基苯胺；邻二甲苯；对硝基甲苯
中图分类号：O621．3 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of 3, 4 - Dimethyl Aniline CUI Kai1, SHEN Hong*2 (1. School of Chemistry & Life Science, Nanjing University Jinling College, Nanjing 210089, China；2. Jiangsu Open University, Nanjing 210036, China), Huaxue Shiji, 2017, 39(7)
Abstract: 3, 4- Dimethyl aniline was prepared by two different methods with the starting materials of o-xylene or p-nitrotoluene. The target product was obtained by the reaction of acylation, oximation, Beckmann rearrangement and hydrolysis from o-xylene. The purity was 99%, and the total yield was 53%. 3, 4- Dimethyl aniline was synthesized by N-(2-methyl-5-nitrobenzyl) acetamide intermediate, and the purity was 99%. The total yield was 50%. The target compounds were confirmed by IR, 1HNMR, MS and elemental analyses.
Key words：3, 4 - dimethyl aniline；o-xylene；p-nitrotoluene
N-[(S)-1-(乙氧羰基)-3-苯丙基]-L-丙氨酸的合成
周勇
（重庆三峡医药高等专科学校附属医院，重庆 404120）
摘要：以苯乙酮和乙醛酸为原料制得3-苯甲酰基丙烯酸乙酯，与L-丙氨酸苄酯对甲苯磺酸盐经迈克尔加成、还原、拆分制得标题化合物，总收率约20%，纯度达99.8%。
关键词：苯乙酮；乙醛酸；N-[(S)-1-(乙氧羰基)-3-苯丙基]-L-丙氨酸；合成
中图分类号：0641.4 文献标识码：A 文章编号：0258-3283（2017）
Synthesis of N-[(S)-1-ethoxycarbonyl-3-phenylpropyl]-L-alanine ZHOU Yong (Subsidiary Hospital of Chong Qing Three Gorges Medical College, Chongqing 404120, China), Huaxue Shiji, 2017, 39(8)
Abstract: N-[(S)-1-ethoxycarbonyl-3-phenylpropyl]-L-alanine was prepared from acetophenone by reaction with glyoxylic acid to obtain ethyl 3-benzoylacrylate, which was subjected to Michael addition with L-alanine benzyl ester tosylate and then reduction. The total yield of the target compound was about 20%, and the purity was 99.8%.
Key words: acetophenone；glyoxylic acid；N-[(S)-1-ethoxycarbonyl-3-phenylpropyl]-L-alanine；synthesis
