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《化学试剂》2017年第12期中英文摘要

发布时间: 2017-12-20 11:29:39   试剂信息网


钙钛矿太阳能电池稳定性研究进展:通向实用的必经之路

邹龙花a,朱英明*a,b,唐思扬b

(四川大学 a. 新能源与低碳技术研究院,b.化学工程学院,四川 成都  610207

 

摘要:钙钛矿太阳能电池是近年来发展最快的光伏技术,但其稳定性研究较少。通过类比光伏产品的生产和使用标准,明确了钙钛矿太阳能电池所需达到的稳定性标准,并在此基础上简要讨论了环境温度、湿度、紫外光等条件下的有机无机杂化钙钛矿吸光材料的稳定性问题及当前解决方案。通过对以上关键问题的讨论和总结,旨在推动钙钛矿太阳能电池材料及器件的稳定性研究和钙钛矿太阳能电池的商业化进程。

关键词:钙钛矿;太阳能电池;稳定性;实用

中图分类号:TK91                文献标识码:A             文章编号:0258-32832017

 

Progress of Stability Research on Perovskite Solar Cells: the Kye of Utilization ZOU Long-huaaZHU Ying-ming*a, b, TANG Si-yangb (a. Institute of New Energy and Low-Carbon Technology, b. School of Chemical Engineering, Sichuan University, Chengdu 610207,China), Huaxue Shiji, 2017, 39(12)

AbstractThe power conversion efficiency record of perovskite solar cells keeps breaking. However, as a promising photovoltaic technology, the perovskite solar cells are unstable. Until now, the standard of perovskite solar cells is lack, so we analogy to the commercial photovoltaic production standards, to which perovskite solar cells may satisfy. We discussed the influence of temperature, humidity, UV-light on the perovskite absorber stability. Through the discussion and summarization of the key issues, we aiming to promote the stability study of perovskite solar cells materials and devices and the commercialization of perovskite solar cells.

Key wordsperovskite solar cell; solar cells; stability; utilization

 

 

2-羟基萘-1-甲醛Cu(II)配合物的合成、晶体结构和抗菌活性

王大伟1a, 1b,周林宗2,杨思林1b,何子康1a,史正军*1a

1. 西南林业大学 a. 生命科学学院,b. 教务处,云南 昆明  650224

2. 楚雄师范学院 地理科学与旅游管理学院,云南 楚雄  675000

 

摘要:在水热条件下合成了一种新的Cu(II)配合物[Cu(nap)2],配合物的分子结构通过X-射线单晶衍射确认,并用元素分析、红外光谱、紫外光谱法对配合物进行了表征。晶体结构分析表明,配合物[Cu(nap)2]为单斜晶系,P21/c空间群,a = 5.7359(9) Å,b = 5.4715(8) Å,c = 25.954(4) Å,β = 95.300(2)°,V = 811.06(2) Å3Z = 2。中心Cu(II)离子与4个氧原子采取平面正方配位构型,而且分子内所有原子均在同一个平面内,晶体中相邻两层平面的分子之间存在着边对边ππ相互作用,并以此组装成折叠层状三维超分子结构。另外,以有害真菌稻疫为对象,研究了在相同浓度下配体、金属盐及铜配合物对稻疫真菌的离体抗菌活性。结果显示,配合物[Cu(nap)2]比配体nap和Cu(OAc)2·H2O具有更强的抑菌活性。

关键词:铜配合物;无机合成;单晶结构;抗菌活性

中图分类号:O614.24        文献标识码:A             文章编号:0258-32832017

 

Synthesis, Crystal Structure and Antifungal Activities of Cu(II) Complex Based on 2-Hydroxynaphthalene-1-carbaldehyde WANG Da-wei1a,1b, ZHOU Lin-zong2, YANGSi-lin1b, HEZi-kang1a, SHIZheng-jun*1a (a. School of Life Science, b. Office of Academic Affairs, Southwest Forestry University, Kunming 650224, China; 2. School of Geographical Science and Tourism Management, Chuxiong Normal University, Chuxiong 675000, China)

Abstract: A new Cu(II) complex, [Cu(nap)2] was synthesized by the reaction of Cu(OAc)2 with 2-hydroxynaphthalene-1-carbaldehyde (nap) under hydrothermal conditions, and the crystal structure was determined by single crystal X-ray diffraction. Then the complex was confirmedby elemental analysis, IR and UV spectroscopy. The crystal structure shows that the complex [Cu(nap)2] crystallizes in monoclinic, P21/c space group, with a = 5.7359(9) Å, b = 5.4715(8) Å, = 25.954(4) Å, β = 95.300(2)°, V = 811.1(2) Å3, Z = 2. The central Cu(II) ion adopt square plane coordination geometry with four oxygen atoms, and all the atoms of [Cu(nap)2] molecule are in the same plane. Between the two adjacent layer π···π interactions were observed, and by which the complexes further extended into stable 3D supramolecular framework. In addition, the title complex and ligand were screened for antifungal activities against Phytophthorafragariae fungi using the mycelial growth rate method, and complex [Cu(nap)2] shows more antifungal activity than nap and Cu(OAc)2·H2O at the same concentration.

Key words: Cu complex; inorganic synthesis; single crystal structure; antifungal activity



黄酮C-7接枝氧肟酸的合成及尿素酶抑制活性研究

师维康,刘琦,倪伟伟,龚思华,刘文润,徐宁,李腾飞,孙玉文,李玲霞,肖竹平*

(吉首大学 化学化工学院 武陵山地区民族药解析与创新湖南省工程实验室,湖南 吉首 416000)

 

摘要:某些天然黄酮具有尿素酶抑制活性,为强化黄酮类化合物的尿素酶抑制作用,通过烷基化、肟化等方法对7-羟基黄酮、白杨素、刺芒柄花素和大豆苷元进行了接枝衍生,分别用1HNMR、MS等方法对其进行结构验证,并研究其尿素酶抑制活性。活性测定表明,部分化合物对尿素酶具有较强的抑制活性,强于阳性对照乙酰氧肟酸。其中,4ʹ-羟基异黄酮-7-基-O-乙酰氧肟酸的IC50 = 6.21(±0.82)μmol/L。

关键词:黄酮;结构改造;氧肟酸;幽门螺旋杆菌;尿素酶抑制剂

中图分类号:R914.5       文献标识码:A         文章编号:0258-3283(2017)

 

Synthesis and Evaluations of Flavonoid Containing Hydroxamic Acids as Urease Inhibitors SHI Wei-kang, LIU Qi, NI Wei-wei, GONG Si-hua, LIU Wen-run, XU Ning, LI Teng-fei, SUN Yu-wen, LI Ling-xia, XIAO Zhu-ping*(Hunan Engineering Laboratory for Ethnomedicine of Wuling Mountains, College of Chemistry and Chemical Engineering, Jishou University, Jishou 416000, China), Huaxue Shiji, 2017, 39(12)

Abstract:Some natural flavonoids have urease inhibitory activity. In order to strengthen the urease inhibition of flavonoids, 7-hydroxyflavone, chrysin, formononetin and daidzein have been investigated by alkylation and oximation. The structures of these compounds were confirmed by 1HNMR, MR, and their urease inhibitory activities were investigated. The activity assay showed that some of the compounds had strong inhibitory activity on urease, which was stronger than that of positive control AHA. Where S4 IC50 reached 6.21 (±0.82) μmol/L.

Key words:Flavonoids; structural modification; acetohydroxamic acid; Helicobacter-pylori; Urease inhibitor



二氢三嗪类化合物的设计、合成及其促葡萄糖消耗活性研究

罗维,杨宗圯,王建塔,张吉泉,汤磊*

贵州医科大学 药学院,贵州 贵阳  550004

 

摘要:以芳香醛和乙酸乙烯酯为原料,经Aldol羟醛缩合反应得到中间体,再与盐酸二甲双胍反应合成一系列新型结构的标题化合物。其结构经1HNMR、13CNMR和HRMS 确证。在HepG2细胞模型中对目标化合物进行了促葡萄糖消耗活性测试,结果显示大部分化合物具有一定的促葡萄糖消耗活性。其中,化合物4-氨基-3, 6-二氢-2-二甲氨基-6-苯乙烯基-1, 3, 5-三嗪、4-氨基-3, 6-二氢-2-二甲氨基-6-(2, 3-二甲氧基)苯乙烯基-1, 3, 5-三嗪、4-氨基-3, 6-二氢-2-二甲氨基-6-(3, 4-二甲氧基)苯乙烯基-1, 3, 5-三嗪、4-氨基-3, 6-二氢-2-二甲氨基-6-(2, 5-二甲氧基)苯乙烯基-1, 3, 5-三嗪和4-氨基-3, 6-二氢-2-二甲氨基-6-胡椒苯乙烯基-1, 3, 5-三嗪的促葡萄糖消耗活性较阳性对照药二甲双胍略强或相当,它们具有进一步开发的价值。

关键词:二甲双胍;二氢三嗪;合成;葡萄糖消耗活性

中图分类号:R914.5         文献标识码:A        文章编号:0258-32832017

 

Synthesis and Glucose Consumption Activity of Dihydrotriazines LUO Wei, YANG Zong-yi, WANG Jian-ta, ZHANG Ji-quan, TANG Lei*(College of Pharmacy, Guizhou Medical University, Guiyang 550004, China), Huaxue Shiji, 2017, 39(12)

Abstract: Using aromatic aldehydes and vinyl acetate as the starting materials, the key intermediates were synthesized via aldol condensation, which reacted with metformin hydrochloride to afford a novel series of dihydrotriazine derivatives. The structures of the target compounds were confirmed by 1HNMR, 13CNMR and HRMS, and their glucose consumption activity were investigated in human liver cancer HepG2 cell lines. The results showed that most of the synthesized compounds possessed a certain glucose consumption activity. Among them, 4-amino-3, 6-dihydro-2-dimethylamino-6-phenylvinyl-1, 3, 5-triazine, 4-amino-3, 6-hih-ydro-2-dimethylamino-6-(2, 3-dimethoxyl)phenylvinyl-1, 3, 5-triazine, 4-amino-3, 6-dihydro-2-dim-ethylamino-6-(3, 4-dimethoxyl)phenylvinyl-1, 3, 5-triazine,4-amino-3, 6-dihydro-2-dimethylamino-6-(2, 5-dimethoxyl)phenylvinyl-1, 3, 5-triazine and 4-amino-3, 6-dihydro-2-dimethylamino-6-piper-onylphenylvinyl-1, 3, 5-triazineexhibited comparable or more potent activities than the positive control metformin, and thus were worthy of further evaluation.

Key words: metformin; dihydrotriazine; synthesis; glucose consumption activity     

 


基于消除-加成机理β-氨基-β-芳基丙烯醛新合成方法研究

秦剑1,刘雨风1,居辰阳2,李飞龙1,赵敏*1,陈建中*2

(1.华东理工大学 化学与分子工程学院,上海  2002372.上海交通大学 化学化工学院,上海  200240)

 

摘要:研究了α-溴代肉桂醛与苯酚的具体反应过程,证明了其先消除再加成的反应机理,进而将该反应应用于β-芳基丙烯醛的β-位含氮基团官能化反应中。通过易得的α-溴代肉桂醛与邻苯二甲酰亚胺钾盐反应,得到一系列β-含氮官能团芳基丙烯醛,所得产物结构经1HNMR、13CNMR、ESI-MS和IR等表征,构型经单晶确定。β-芳基丙烯醛官能化产物经简单转化即可应用于药物和天然产物的合成中。另外,根据该机理对β-芳基丙烯醛进行其他基团官能化的反应正在进行中。

关键词:消除-加成机理;α-溴代肉桂醛;β-氨基-β-芳基丙烯醛;药物合成

中图分类号:O625; O622.6      文献标识码:A      文章编号:0258-32832017

 

Synthesis of β-Amino-β-arylacroleins Based on Elimination-addition Mechanism QIN Jian1, LIU Yu-feng1, JU Chen-yang2, LI Fei-long1, ZHAO Min*1, CHEN Jian-zhong*2 (1.School of Chemistry and Molecular EngineeringEast China University of Science and Technology, Shanghai 200237, China; 2.School of Chemistry and Chemical EngineeringShanghai Jiao Tong University, Shanghai 200240, China)HuaxueShiji,

Abstract:An elimination-addition pathway for the reaction of α-bromo-β-arylacroleins with phenol has been elucidated. β-Amino-β-arylacroleins have been prepared according to this reaction mechanism. The α-bromo-β-arylacroleins were obtained via bromination with bromine water.  The corresponding β-(1,3-dioxoisoindolin-2-yl)-β-arylacroleins were subsequently prepared with good yields in the presence of potassium 1,3-dioxoisoindolin-2-ide in DMF. The structures were confirmed by 1HNMR, 13CNMR, ESI-MS, IR and X-ray. The β-substituted-β-arylacrylaldehydes could be used for the synthesis of bioactive compounds. In addition, related reactions are currently being investigated according to the mechanism.

Key wordselimination-additionmechanism;α-bromo-β-arylacrylaldehydes;β-amino-β-arylacrylaldehydes;drug synthesis



β, β'-双取代-(E)-甲酸乙烯酯的选择性合成

王兴广a,刘冲a,张振锋* b,张万斌*a, b

(上海交通大学 a. 化学化工学院,b. 药学院,上海  200240)

 

摘要:以廉价易得的各类苯乙酮衍生物为原料,经Wittig-Horner反应得到(E)-β-芳基丙烯酸酯,然后经DIBAL-H还原、MnO2氧化以及Baeyer-Villiger氧化“一锅法”合成一系列具有全新结构的标题化合物。上述产物是一类重要的药物分子和活性产物中间体,其结构通过1HNMR和13CNMR确认。该合成路线简单易行、选择性高,是至今为止获得该类化合物的首例方法学研究报道。

关键词:苯乙酮;甲酸乙烯酯;合成;选择性

中图分类号:O622.5       文献标识码:A      文章编号:0258-32832017

 

Selective Synthesis of β, β'-Disubstituted-(E)-vinyl Formate WANG Xing-guanga, LIU Chonga, ZHANG Zhen-feng*b, ZHANG Wan-bin*a, b(a. School of Chemistry and Chemical Engineering, b. School of Pharmacy, Shanghai Jiaotong University, Shanghai 200240), Huaxue Shiji, 2017, 39(12)

Abstract:(E)-β-Aromatic acrylic esters can be selectively synthesized via Wittig-Horner reaction using commercially available acetophenones and readily transformed to β, β'-disubstituted-(E)-vinyl formate by DIBAL-H reduction, MnO2 oxidation and a Baeyer-Villiger reaction in a sequential process. Such novel structural products are very important intermediates for the preparation of pharmaceuticals and bioactive compounds. This methodology has the advantages of operational simplicity and high selectivity. To the best of our knowledge, this investigation is the only methodology concerning the synthesis of such products with a single configuration.

Key wordsacetophenone; vinyl formate; synthesis; selectivity

 


环保领域石油烃类标准体系存在的问题及建议

张利飞*1,刘昉2,任玥1,刘爱民1,吴忠祥1,黄业茹1,李国刚1

1. 国家环境分析测试中心,北京  1000292. 全国化学试剂信息站,北京  100050

 

摘要:石油烃类是基于方法定义的目标物,在《农用地土壤环境质量标准(三次征求意见稿)》中称为“石油烃总量”,在《地表水环境质量标准》中称为“石油类”。当前,环境质量标准、污染物排放标准和环境监测类标准还存在一些涉及石油烃类的标准体系完善和履行国际公约压力等问题。从石油烃类的概念和发展历程出发,系统梳理了当前各类环保标准中有关石油烃类的现状和存在问题,提出统一石油烃类概念、以“石油烃总量”代替“石油类”修订环境质量标准和排放标准、增加生物法和石油烃标样的研制、加大科研投入和部门协调等完善土壤和水体中石油烃类标准体系的建议。

关键词:石油烃类;环境标准;分析方法;四氯化碳

中图分类号:TQ420.7         文献标识码:A       文章编号:0258-32832017

 

Current Status and Suggestions on Environmental Standards of Petroleum Hydrocarbons ZHANG Li-fei*1, LIU Fang2, REN Yue1, LIU Ai-min1,WU Zhong-xiang1, HUANG Ye-ru1, LI Guo-gang1 (1. National Research Center for Environmental Analysis and Measurement, Beijing 100029, China; 2. Chemical Reagents Information Center of China, Beijing 100050, China), HuaxueShiji, 2017, 39(12)

Abstract: The petroleum hydrocarbons are method-defined analytes. It was defined as total petroleum hydrocarbons and petroleum oil in the soil environmental quality standard for agricultural land and environmental quality standards for surface water in China, respectively. There were problems for petroleum hydrocarbons in some environmental standards, such as quality standards, emission standards, and monitoring standards. Current states on environmental standard are discussed based on various concepts of the petroleum hydrocarbons. Several suggestions were given out to improve the environmental standards system, including unified concept of petroleum hydrocarbons, to revise environmental standards using total petroleum hydrocarbons, to develop biological methods and standard solutions, and to increase financial input and sectoral coordination.

Key words: petroleum hydrocarbons; environmental standard; analytical method; carbon tetrachloride

 


查尔酮类化合物抗糖尿病活性研究进展

朱盼虎,胡孟奇,李家明*,杨雨

(安徽中医药大学 药学院, 安徽 合肥  230038)

 

摘要:查尔酮类化合物是一类存在于药用植物中的天然有机化合物,具有抗糖尿病、抗肿瘤、催眠、抗菌、抗病毒、抗痛风、抗炎等多种生物活性,因此人们对此类化合物进行了大量研究。了解该类化合物的药理作用机制和构效关系,可为新药设计和开发提供先导化合物或药物资源。综述了查尔酮结构改造与修饰及查尔酮衍生物在抗糖尿病活性方面的研究进展。

关键词:查尔酮;先导化合物;糖尿病;活性

中图分类号:R9     文献标识码:A             文章编号:0258-32832017

 

Progress of Anti-diabetes Activity of Chalcone Compounds ZHU Pan-hu, HU Meng-qi, LI Jia-ming, YANG Yu (College of Pharmacy, Anhui University of Chinese Medicine, Hefei 230038)

Abstract:Chalconeisa class of natural organic compounds widely existing in plants, biological activity of anti-diabetes, anti-cancer, hypnotic, anti-bacterial, anti-viral, anti-gout, anti-inflammatory and so on. Therefore, a large amount of researcheshave been done for this type of compounds, understanding the pharmaco-logical mechanisms and the structure-activity relationships of chalcones may provide lead compounds and drug-seeking sources for new drug design and development. The recent advances in structural modification of chalcones and anti-diabetes bioactivities of chalcones derivatives were reviewed.

Key words: Chalcones; lead compounds; diabetes; activity


GSHCTAB功能纳米金比色法快速检测Pb2+的研究 

寇莹莹*,任相浩

(北京建筑大学 城市雨水系统与水环境教育部重点实验室,北京  100044

 

摘要:利用谷胱甘肽(GSH)和十六烷基三甲基溴化铵(CTAB)修饰的功能纳米金GSH-GNPs和CTAB-GNPs对水中的重金属污染物Pb2+进行比色法快速检测,并通过TEM和UV-Vis对其进行表征。结果发现,GSH-GNPs粒径为6.0 nm,浓度为1.5 nmol/L;CTAB-GNPs粒径为9.0 nm,浓度为2.6 nmol/L。两者的最低检出限分别为30 μmol/L和0.5 μmol/L。相对来说,CTAB-GNPs的灵敏度较高,但是GSH-GNPs的制备和检测更为简单。

关键词:功能纳米金;检测;铅离子

中图分类号: O657.3               文献标识码:A 

Rapid Detection of Pb2+ by GSH and CTAB Functionalized Gold Nanoparticles KOU Ying-ying*, REN Xiang-hao (Key Laboratory of Urban Stormwater System and Water Environment, Beijing University of Civil Engineering and Architecture, Beijing 100044)

Abstract: Glutathione (GSH) and 16 alkyl three methyl bromide (CTAB) modified gold nanoparticles GSH-GNPs  and CTAB-GNPs were designed. They were used for the rapid colorimetric detection of heavy metals of lead ions in water. The samples were characterized by TEM and UV-Vis. The particle size of GSH-GNPs was about 6.0 nm with a concentration of about 1.5 nmol/L, and the particle size of CTAB-GNPs was about 9.0 nm with a concentration of about 2.6 nmol/L. The lowest detection limit of GSH-GNPs and CTAB-GNPs was 30 μmol/L and 0.5 μmol/L. The sensitivity of CTAB-GNPs is higher than that of GSH-GNPs, but the preparation and detection of GSH-GNPs is simpler.

Key words: functional gold nanoparticles; detection; lead ion

 

液相色谱-串联质谱技术检测多种基质中的三聚氰胺及10种真菌毒素

刘韬1,张勋*1,王宁1,高杰2,李婷婷2,杨璐1,付瑶1,王佳慧1,张鑫1,邢燕燕1

1. 吉林出入境检验检疫局,吉林 长春  130062

2. 长春理工大学 化学与环境工程学院,吉林 长春  130022

 

摘要:采用QuEChERS方法,建立了液相色谱-串联质谱法测定粮谷(大米、小米、高粱米、小麦、黑米、燕麦、玉米、糙米)和饲料中三聚氰胺及10种真菌毒素(FB1、FB2、AFB1、AFB2、AFG1、AFG2、OTA、ZEA、DON、T-2毒素)的分析方法。讨论了提取溶剂和提取体积对回收率的影响,并对液相色谱条件和质谱条件进行了优化,该方法的定量限在0.5 ~ 20 μg/kg之间,不同基质不同浓度的加标回收率在79.2% ~ 92.2%之间(添加水平分别为1倍、2倍和10倍定量限,n = 6),相对标准偏差<5.7%。

关键字:QuEChERS方法;三聚氰胺;真菌毒素;液相色谱-串联质谱法

中图分类号:TQ450.7        文献标识码:A         文章编号:0258-32832017

 

Determination of Eleven Mycotoxins from Various Matrixes by Liquid Chromatography-tandem Mass Spectrometry LIU Tao1, ZHANG Xun*1, WANG Ning1, GAO Jie2, LI Ting-ting2, YANG Lu1, FU Yao1, WANG Jia-hui1, ZHANG Xin1, XING Yan-yan1 (1.Jilin Entry-Exit Inspection and Quarantine Bureau, Changchun 130062, China; 2. College of Chemistry and Environmental Engineering, Changchun University of Science and Technology, Changchun 130022, China), Huaxue Shiji, 2017, 39(12)

AbstractAn analytical method of melamine and ten mycotoxins (FB1, FB2, AFB1, AFB2, AFG1, AFG2, OTA, ZEA, DON, T-2)has been developed for the determination of cereal grains(rice, millet, sorghum rice, wheat, black rice, oats, corn, brown rice)and feed stuff by liquid chromatography-tandem mss spectrometry. The influence on recovery of extract solvent and volume had been discussed. And the performance liquid chromatography (HPLC) conditions and mass spectrometer conditions had been optimized. The limits of detection of method were 0.5 20 μg/kg for different compounds, recoveries of different matrixes and concentrations ranged from 79.2% 92.2% at the spiked levels of quantitative restrictions of one, two times and ten times, and the relative standard deviations were less than 5.7%(n = 6).

Key wordsQuEChERS method; melamine ;mycotoxins; gas chromatography-mass spectrometry



气相色谱法检测驱蚊环、驱蚊贴中化学驱蚊成分

蒋莹*,肖峥,李海燕,邵秋凤,周丽佳

(上海市质量监督检验技术研究院,上海  201114)

 

摘要:旨在建立一种分析方法,以测定近年来市场上出现的驱蚊环、驱蚊贴等新型驱蚊产品中可能存在的避蚊胺、驱蚊酯、羟哌酯等化学驱蚊成分。确立了超声萃取的前处理方法、气相色谱法(火焰离子化检测器)的色谱条件,以邻苯二甲酸二戊酯为内标物的内标定量方法。该方法前处理过程简便、线性和重复性良好,检出限<0.01%,能够满足检测要求。通过对94个实际样品的测定,证明该方法具有较好的实用性。

关键词:气相色谱法;驱蚊环;驱蚊贴;避蚊胺;驱蚊酯;羟哌酯

中图分类号:R184.31               文献标识码:A              文章编号:0258-32832017

 

Detection for Chemical Mosquito Repellent in Anti-mosquito Wristbands and Stickers by Gas Chromatography JIANG Ying*, XIAO Zheng, LI Hai-yan, SHAO Qiu-feng, ZHOU Li-jia(Shanghai Institute of Quality Inspection and Technical Research, Shanghai 200114, China), Huaxue Shiji, 2017, 39(12)

Abstract: The method was established to detect the possible chemical mosquito repellent (DEET, BAAPE, Bayrepel, etc) in anti-mosquito wristbands and stickers which were available in the market recently. The detection was done with pretreatment method of ultrasonic extraction, detection method of gas chromatography with FID detector and internal standard quantitative method with diamyl phthalate as internal standard. The method meets the test requirements, based on the advantages of simple pretreatment process, good linearity and repeatability, detection limit less than 0.01%.The detection results of 94 samples show that this method has good practicability.

Key words: gas chromatography; anti-mosquito wristband; anti-mosquito sticker; diethyltoluamide (DEET); insectifugeEster(BAAPE); bayrepel


基于溴化氢诱导下纳米金氧化刻蚀比色法检测六价铬

贵莉莉

(新乡职业技术学院,河南 新乡  453000)

 

摘要:设计了一种基于纳米金被六价铬氧化刻蚀的高敏感、高专一性的比色传感器来检测六价铬。当溴化氢存在时,由能斯特方程得到Cr6+/Cr3+的标准电势高于Au+/Au的标准电势。因此,当六价铬存在时,纳米金被刻蚀成小粒径的纳米粒子,导致在520 nm处的吸光度不断降低,650 nm处的吸光度则不断增大。六价铬的浓度在0.1 ~ 100 μmol/L范围内,对数值与吸光度变化值呈良好的线性关系,线性方程为y = 0.08332x+0.08286,相关系数R为0.99,检出限为0.06 μmol/L,其他金属离子几乎不存在干扰。本方法用于自来水样品中六价铬的测定,实验结果令人满意。

关键词:纳米金;溴化氢;六价铬;氧化刻蚀;比色

中图分类号:O65        文献标识码:A         文章编号:0258-32832017

 

Colorimetric Detection of Cr(VI) Based on the Oxidation Etching of Gold Nanoparticles GUI Li-li(        , Xinxiang Vocational and Technical College, Xinxiang 453000, China), Huaxue Shiji, 2017, 39(12)

Abstract: A highly sensitive and specific colorimetric sensor for Cr(VI) detection based on the oxidation etching of gold nanoparticles by Cr(VI) was designed. In the presence of hydrogen bromide, based on the Nernst equation, the electron potential of Cr(VI)/Cr(III) is higher than that of Au(I)/Au(0). Thus, the gold nanoparticles are etched to nanoparticles with smaller particle size, which leads to the gradual decrease of the absorbance value at 520 nm, and the gradual increase of the absorbance value at 650 nm. There is a good linear relationship between the absorbance change and the logarithm of the Cr(VI) concentrations in the range of 0.1 ~ 100 μmol/L, its regression equation is y = 0.08332x+0.08286, and the correlation coefficient is 0.99, with a low detection limit of 0.06 μmol/L, and there is almost no interference from other metal ions. The method is applied to the detection of Cr(VI) in tap water, the results are satisfactory.

Key words: gold nanoparticles; hydrogen bromide; hexavalent chromium; oxidation etching; colorimetric



ICP-OES法同时测定L-半胱氨酸盐酸盐产品中的7种杂质元素

郑琦,方诚,凌芳*,陈浩云,肖历

(国药集团化学试剂有限公司,上海  200002

 

摘要:研究了电感耦合等离子原子发射光谱仪法(ICP-OES)测定L-半胱氨酸盐酸盐中的7个杂质元素(Ca、Co、Fe、K、Mg、Na、Zn)的方法,确定了最佳分析谱线以及仪器的工作条件,分析了过程中存在的干扰。所用实验方法加标回收率为98.16% ~ 104.4%,测得杂质浓度值的标准偏差RSD<7%。因此,该方法回收率不仅高,同时具有较低的检出限和较好的精密度。

关键词:ICP-OES;L-半胱氨酸盐酸盐;干扰

中图分类号:TQ460.7     文献标识码:A      文章编号:0258-32832017

 

Simultaneous Determination of 7 Impurity Elements in L-Cysteine Hydrochloride with ICP-OES ZHENG Qi, FANG Chen, LING Fang*, CHEN Hao-yun, XIAO LiSinopharm Chemical Reagent Co., Ltd, Shanghai 200002, China, Huaxue Shiji, 2017, 39(12)

Abstract: This work has investigated the determination method of the impurities(Ca, Co, Fe, K, Mg, Na, Zn) in L-cysteine hydrochloride via ICP-OES. The best spectral lines, working conditions, interference existing in the process has been elucidated. The experimental recovery rate of this method is 98.16% ~ 104.4%, and the standard deviation of the impurity concentration is RSD <7%. Therefore, the recovery rate is high, and detection limit and precision is fine.

Key words: ICP-OES; L-cysteine hydrochloride; interference

 

水中阴离子表面活性剂测定方法的对比研究

                              郭晋君*,刘建利,宋蓓

(陕西省环境监测中心站,陕西 西安  710054

 

摘要:用连续流动分析仪测定水样中阴离子表面活性剂,结果表明:线性良好,相关系数可达0.9997,检出限可低至0.02 mg/L;测定标准溶液,相对标准偏差在1.2% ~ 4.0%之间,精密度良好;实际水样的加标回收率范围为93.0% ~ 106%,准确度良好。将该方法与国标方法进行比较,结果显示两种方法无显著差异。

关键词:连续流动分析;阴离子表面活性剂;对比研究

中图分类号:O661.1      文献标识码:A       文章编号:0258-32832017 

Determination of Anionic Surfactants in Water GUO Jin-jun*, LIU Jian-li, SONG Bei (Shaanxi Environmental Center Monitoring StationXian 710054, China)

AbstractThis work determined the anionic surfactants in water by continuous flow analysis, the results showed that the good linear regression, the correlation coefficient was 0.9997, and the detection limit was 0.02 mg/L. Determination of standard samples by continuous flow analysis, the relative standard deviation between 1.2% ~4.0%, the precision was good. The recovery rate of water samples was 93.0% ~ 106%, the accuracy was good. The method of continuous flow analysis compared with national standard method, the results showed that two methods had no significant difference.

Key wordscontinuous flow analysis(CFA); anionic surfactants; comparative study


苯酚纯度标准物质的定值及不确定度分析

陈怡,邓超,张辉*

(浙江省计量科学研究院,浙江 杭州  310013

 

摘要:建立了苯酚纯度标准物质的定值和不确定度评定方法。通过气相色谱-质谱法和傅里叶变换红外光谱法进行定性分析。为了提高定值准确度,同时采用了质量平衡法(MB)和差示扫描量热法(DSC)进行定值分析,其中质量平衡法包括高效液相色谱面积归一化法(HPLC-AN)、气相色谱面积归一化法(GC-AN)、水分、溶剂残留和灰分分析。运用HPLC法进行了均匀性检验和稳定性考察。分别建立MB和DSC方法的测量模型,根据不确定度传播率推导和计算各个不确定度分量和合成标准不确定度,定值结果为99.42%,相对拓展不确定度为0.20%(k = 2)。该标准物质对于化妆品等基体中苯酚的量值传递和量值溯源具有重要意义。

关键词:标准物质;苯酚;高效液相色谱;气相色谱归一化法;质量平衡法;差示扫描量热法;不确定度

中图分类号:O625            文献标识码:A            文章编号:0258-32832017

 

Purity Determination and Uncertainty Evaluation of Phenol Reference Material CHEN Yi, DENG Chao, ZHANG Hui* (Zhejiang Provincial Institute of Metrology, Hangzhou 310013, China), Huaxue Shiji, 2017, 39(12)

Abstract: The approach for purity determination and uncertainty evaluation of phenol reference material was established. The qualitative analysis was performed via the gas chromatographic mass spectrometry (GC-MS) and fourier transform infra redspectroscopy (FT-IR), while the quantitative analysis was carried out by means of differential scanning calorimetry (DSC) and balance method (MB) simultaneously, by which the accuracy of purity result was supposed to be enhanced. The MB method was based on area normalization methods of both high performance liquid chromatography (HPLC-AN) and gas chromatography (GC-AN) as well as impurity assessment. The uniformity and stability of phenol reference material was investigated by HPLC. The determination of uncertainty components and the combined standard uncertainty were accomplished by establishment of the measurement models involving both MB method and DSC, followed by derivation and calculation of formulas on basis of uncertainty spreading rate. The purity determined in this way was 99.43% with the relative standard uncertainty of 0.25% (k = 2). The reference material was of great significance in view of quantity transfer and value traceability.

Keywords: reference material; phenol purity determination uncertainty; high performance liquid chromatography; gas chromatography; differential scanning calorimetry

 

蚓粪生物炭对亚甲基蓝的吸附性能研究

郭丰艳*,马文庆,李拓,刘广鑫

(唐山学院 环境与化学工程系,河北 唐山  063000)

 

摘要:蚯蚓粪便经400 ℃慢速热解2 h制成蚓粪生物炭(VB),VB经一定浓度硝酸处理得到氧化后的生物炭(OVB)。采用SEM和红外光谱对VB、OVB的形貌及表面官能团进行表征。以VB、OVB为吸附剂,研究了两者对亚甲基蓝染料的吸附性能。实验结果表明,VB、OVB对亚甲基蓝的吸附量随着亚甲基蓝初始浓度、吸附时间和吸附温度的增加而增大。Langmuir模型对VB、OVB吸附亚甲基蓝的拟合结果较好,拟合相关系数分别为0.97809和0.99262,表明该吸附主要为单分子层吸附,吸附动力学符合二级动力学方程。

关键词:蚓粪生物炭;亚甲基蓝;吸附

中图分类号:O647.3         文献标识码:A          文章编号:0258-32832017

 

Adsorption Capacity of Vermicompost Biochar for Methylene Blue GUO Feng-yan*, MA Wen-qing, LI Tuo, LIU Guang-xinDepartment of Environmental and Chemical Engineering, Tangshan University, Tangshan 063000, China, Huaxue Shiji, 2017, 39(12)

Abstract: Vermicompost was carbonized by pyrolysis to produce vermicompostbiochar (VB) at temperature of 400 ℃ and residence time 2 h. VB was oxidized by nitric acid to get oxidizedvermicompostbiochar (OVB). Pore structure and surface functional group of VB and OVB were characterized by SEM and infrared spectrometry. Adsorption capacity of VB and OVB for methylene blue were investigated. The result showed that increase of initial concentration of methylene blue, adsorption time and temperature brought about rise of adsorption amount. The Langmuir adsorption isotherms model can well describe the adsorption process (R2VB=0.97809, R2OVB=0.99262). Adsorption of VB and OVB for methylene blue is monolayer absorption. The adsorption kinetic can be well simulated by second order model.

Key words: vermicompostbiochar; methylene blue; adsorption

 

罗丹明型Cu2+比色探针的合成及识别

田怡,陈稼轩*,王红艳,赖琪琪

(乐山师范学院 化学学院,四川 乐山  614000)

 

摘要:以偶氮苯水杨醛和罗丹明B-酰肼为原料,经缩合反应得到Cu2+比色探针RAH,其结构经1HNMR、MS和元素分析表征。通过紫外-可见光谱法研究了RAH对金属离子的识别能力。结果表明,RAH在CH3CN/Tris-HNO3溶液中对Cu2+具有高选择性识别能力,溶液由无色迅速转变为紫红色,与Cu2+形成1 : 1型配合物,结合常数为1.1×105 dm3/mol。

关键词:罗丹明B;比色探针;Cu2+;识别

中图分类号:O657.3              文献标识码:A             文章编号: 0258-3283(2017)

 

Synthesis and Recognition of a Novel Rhodamine Based Cu2+ Colorimetric Probe  TIAN Yi,  CHEN Jia-xuan*, WANG Hong-yan, LAI Qi-qi (Department of Chemistry, Leshan Normal University, Leshan 614000, China), Huaxue Shiji, 2017, 39(12)

Abstract:A novel Cu2+ colorimetric probe RAH was synthesized by condensation reaction of azobenzene salicylaldehyde and Rhodamine B hydrazide, and its structure was confirmed by 1HNMR, MS and elemental analysis. The recognition properties of RAH with metal ions have been investigated by the UV-Vis spectrophotometry. The results showed that the probe RAH exhibits high selectivity and sensitivity to Cu2+ in CH3CN/Tris-HNO3 solution with an obvious color change from colorless to pink. The interaction of Cu2+ and probe RAH was proven to adopt a 1 : 1 binding stoichiometry and the binding constant was 1.1×105 dm3/mol.

Key wordsRhodamine B; colorimetric probe; Cu2+; recognition



十六烷基三甲基溴化铵-羧甲基纤维素离子复合物的胶束性质研究

吴平*,魏海杰

(吉林化工学院 化学与制药工程学院,吉林 吉林  132022

 

摘要:十六烷基三甲基溴化铵通过静电相互作用与羧甲基纤维素形成离子复合物胶束。电导率法测定离子复合物的最低聚集浓度为2.42×10-4 mol/L。表面活性剂浓度达到聚电解质等电点时,复合物从溶液中析出沉淀。甲基橙的最大吸收波长发生蓝移,证明在复合物溶液中存在胶束的疏水结构。复合物粒径在环糊精加入后减小,溶液透过率增加。

关键词:羧甲基纤维素;聚电解质;环糊精;静电作用

中图分类号:O636.1         文献标识码:A             文章编号:0258-32832017

 

Micellar Properties of Ionic Complex of Carboxyl Methyl Cellulose and Hexadecyl Trimethyl Ammonium Bromide WU Ping*, WEI Hai-jie(School of Chemistry and Pharmaceutical Engineering, Jilin Institute of Chemical Technology, Jilin 132022, China), Huaxue Shiji, 2017, 39(12)

Abstract: Carboxymethyl cellulose and hexadecyltrimethyl ammonium bromide (cationic surfactant) formed ionic complex by electrostatic interaction. The minimum concentration of the ionic complex was 2.42×10-4 mol/L determined by conductimetric method. With the concentration of the surfactant increasing at the isoelectric point of polyelectrolyte, the polymer precipitated from the solution. The maximum of adsorption wave number of methyl orange in complex solution showed blue shift, which proved the hydrophobic structure of micellar in complex solution. With the addition of cyclodextrins, the particle size of polymer decreased and the transmissivity of the solution increased.

Key words: carboxymethylcellulose; polyelectrolyte; cyclodextrins; electrostatic interaction

 


手性流动相添加剂法拆分辛弗林对映体

翟明翚,于浩,刘呈利,孟培,苏立强*

(齐齐哈尔大学 化学与化学工程学院,黑龙江 齐齐哈尔  161006)

 

摘要:建立了高效液相色谱手性流动相添加剂法拆分辛弗林对映体的方法。选用C18色谱柱,以0.5 g/L羧甲基-β-环糊精(CM-β-CD)为添加剂,流动相为混合液(V(乙腈)︰V(甲醇)︰V(水) = 70 : 15 : 15),紫外检测波长为202 nm,流量为0.2 mL/min,pH 4.20。在此条件下,辛弗林对映体分离度为1.47。

关键词:高效液相色谱;手性流动相添加剂;拆分;辛弗林对映体

中图分类号:O657.7              文献标识码:A             文章编号:0258-32832017

 

Resolution of Synephrine Enantiomeric Using Chiral Mobile Phase Additive ZHAI Ming-hui, YU Hao, LIU Cheng-li, MENG Pei, SU Li-qiang*(College of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, China), Huaxue Shiji, 2017, 39(12)

Abstract: The enantiomeric separation of synephrine by HPLC with chiral mobile phase additive was established. The C18 column was used as stationary phase, using the 0.5 g/L carboxymethyl-β-cyclodextrin(CM-β-CD)as chiral mobile phase additive, and a mixture of acetonitrile-methanol-water(mixed in the ratio of 70 : 15 : 15 by vol.)was used as mobile phase, the UV detection wavelength was set at 202 nm, at a flow-rate of 0.2 mL/min, pH 4.20. Under the optimized conditions, the resolution of synephrine enantiomer was 1.47.

Key word: HPLC; chiral mobile phase additive; separation; synephrine enantiomer


N-苯基硫脲衍生物合成的新方法

刘海灵*,刘媛,王香凤,徐海燕

(北京师范大学 分析测试中心,北京  100875)

 

摘要:硫脲衍生物是一类具有强烈生理和药理活性的有机试剂。使用乙酰乙酰苯胺和硫氰酸铵为原料,在无催化剂的条件下,开发了一条合成标题化合物的方法。结果表明,乙酰乙酰苯胺无论是具有吸电子取代基还是给电子取代基,反应都可以顺利进行。合成了11种硫脲衍生物,所得产物的分离产率为81% ~ 94%,并利用质谱、核磁共振波谱、红外光谱对所合成的化合物进行了表征。

关键词:乙酰乙酰苯胺;硫氰酸铵;N-苯基硫脲衍生物

中图分类号: O622.7               文献标识码:A             文章编号:0258-32832017

 

Synthesis of N-Phenylthiourea Derivatives LIU Hai-ling*, LIU Yuan, WANG Xiang-feng, XU Hai-yan (Analytical & Testing Center, Beijing Normal University, Beijing 100875, China), Huaxue Shiji, 2017, 39(12)

Abstract:Thiourea derivatives are a class of organic reagents possessing important biological and pharmaceutical activities. In this work, a catalyst-free method for the synthesis of N-phenylthiourea derivatives was developed directly from acetoacetanilides and ammonium thiocyanate. Investigation of representative acetoacetanilides demonstrates that the transformation is feasible whether the substituents are electron-donating or electron-withdrawing groups. The desired N-phenylthiourea derivatives were obtained with 81% ~ 94% isolated yields and confirmed by MS, NMR and IR.

Key wordsacetoacetanilides; ammonium thiocyanate; N-phenylthiourea derivatives

 


多果定的合成新工艺

李雪莲1*孙毓韬1张頔2刘长春1周蔚然1

1.常州工程职业技术学院化工学院,江苏常州213164; 2.常州工程职业技术学院实验实训教学部,江苏常州213164)

 

摘要:通过选择盐酸胍和氯代十二烷为原料,两步反应制得标题化合物,并确定最佳合成工艺是无水乙醇为溶剂,盐酸胍和氯代十二烷用量分别为0.1mol和0.15mol,回流反应10h。冷却析出产物,甲苯重结晶得中间体;再以甲苯为溶剂,滴加20%的氢氧化钠溶液中和该中间体,接着与冰醋酸成盐制得,液相质量含量98.0%,收率为95.1%。

关键词:多果定;合成;盐酸胍;氯代十二烷

中图分类号:TQ45          文献标识码:A


Synthesis of DodinzLI Xue-lian1* , SUN Yu-tao1 , ZHANG Di2, LIU Chang-chun1, ZHOU Wei-ran1(1.School of Chemical Engineering, Changzhou Vocational Institute of Engineering, Changzhou213164, China 2. Dept. of Experimental Teaching, Changzhou Vocational Institute of Engineering, Changzhou213164, China),Huaxue Shiji,2017, 39(11),~

Abstract: In this work,guanidine hydrochloride and chlorinated dodecane areselected as raw materials, and the optimum synthesis process was determined by two-step reaction. Use anhydrous ethanol as solvent, mix guanidine hydrochloride (0.1mol) and chlorinated dodecane (0.15mol), after refluxing and stirring for 10h, the mixture was cooled to give the intermediate and recrystallized by toluene. Take toluene as solvent, drop the 20% sodium hydroxide solution to neutralize the intermediate, then form the salt with acetic acid. HPLC content is 98.0% and the yield of 95.1%.

Key words: dodine; synthesis; guanidine hydrochloride; chlorododecane

 


二萜合酶标记底物的设计与合成

郭留城*1,杜利月1,孟瑾1,解丽芹2,李景华3,金少举1

(1. 漯河医学高等专科学校 药学系,河南 漯河  4620022. 新乡医学院 纳米生物医用材料重点实验室,河南 新乡  4530033. 河南大学 天然药物与免疫工程重点实验室,河南 开封  475004)

 

摘要:从二萜类天然产物Cyclooctatin的环化机理猜想出发,设计[2-2H]GGDP(GGDP:香叶基香叶基焦磷酸)、[9-2H2]GGDP、[14-2H]GGDP 等氘带底物,以供研究二萜合酶环化反应机理,并设计[2-F]GGDP氟代底物用于与酶的共结晶研究,以验证猜想的正确性。均以反式-反式金合欢醇为起始原料,分别利用乙酰乙酸甲酯双负离子和单负离子偶联的方法实现碳链的延长,完成了[2-2H]GGDP和[2-F]GGDP的合成工作。在[2-2H]GGDP合成中,β-酮酸酯经D2O交换在C-2位,引入氘原子;在[2-F]GGDP合成中,与乙酰乙酸甲酯单负离子偶联后经Krapcho脱羧反应和Horner-Wadsworth-Emmons反应在C-2位引入F原子。该研究为[9-2H2]GGDP[14-2H]GGDP的合成积累了经验,也为后续进一步研究酶环化反应机制奠定了基础。

关键词:二萜合酶;酶环化反应;标记底物

中图分类号:O624.33            文献标识码:A          文章编号:0258-32832017

 

Design and Synthesis of Labeled Substrates of Diterpene Synthase GUO Liu-cheng*1, DU Li-yue1, MENG Jin1, XIE Li-qin2, LI Jing-hua3, JIN Shao-ju1(1. Department of Pharmacy, Luohe Medical College, Luohe 462002, China2. Institute of Nano-Biomedical Materials, Xinxiang Medical University, Xinxiang 453003, China3. Key Lab of Natural Medicine and Immunal Engineering, Henan University, Kaifeng 475004, China), Huaxue Shiji, 2017, 39(12)

Abstract: Starting from supposition of the cyclization mechanism of cyclooctatin, enzymatic cyclization reaction was designed using deuterium-labeled substrates include [2-2H]GGDP, [9-2H2]GGDP and [14-2H]GGDP. The fluoride-labeled GGDP for cocrystallization was also designed to check the conjecture′s veracity. In this work, the synthesis of [2-2H]GGDP and [2-F]GGDP was completed and farnesol served as the starting material. Dianion and anion generated from methyl acetoacetate coupled with farnesyl bromide to achieve the carbon chain elongation respectively. During the synthesis of [2-2H]GGDP, β-keto ester was exchange labeled in 2H2O to introduce D atom in C-2 position, while to afford [2-F]GGDP Krapcho decarboxylation was applied after the coupling with anion generated from methyl acetoacetate and Horner-Wadsworth-Emmons reaction was utilized to introduce F atom in C-2 position. In this work, experience of synthesis of [9-2H2]GGDP, [14-2H]GGDP was accumulated, and also laid the foundation for further study on the mechanism of the enzymatic cyclization reaction.

Key words: diterpene synthase; enzymatic cyclization reaction; labled substrate


玫红酸的合成研究

胡辰飞,王晓东,刘嵩,王家濬,刘振荣*

(天津市科密欧化学试剂有限公司,天津 300350

 

摘要:在分析化学中,玫红酸是一种重要的酸碱指示剂,应用广泛。但其合成方法存在很大缺陷,工业化生产难度较高。通过大量的文献查阅和实验创新,本文开发出一种新的玫红酸合成方法。以苯酚和四氯化碳为原料,在催化剂作用下加热回流,经取代反应得到产物玫红酸。研究了催化剂和反应时间对反应的影响,得到最佳反应条件:以无水氯化锌为催化剂,135℃回流反应18h。所得产物结构经ESI-MS进行表征。

关键词:四氯化碳;苯酚;玫红酸;合成

中图分类号:O625.14          文献标识码:A           文章编号:0258-3283(2017)

 

Synthesis of AurinHU Chen-fei,WANG Xiao-dong,LIUSong,WANGJia-jun,LIU Zhen-rong*(Tianjin Kermel Chemical Reagent Co.,Ltd.,Tianjin 300350,China)

Abstract: In the analysis of chemistry, the aurin is an important indicator of ph, and it is widely applied.But its synthetic methods are very flawed, and industrial production is more difficult. Through extensive literature review and experimental innovation, this article has developed a new method of synthesis of aurin. With phenol and carbon tetrachloride as raw material, heating reflux, under the action of a catalyst by the substitution reaction product rosolic acid. The effects of catalyst and reaction time on the reaction were elucidated and optimal reaction conditions were obtained. The optimum conditions were anhydrous zinc chloride as catalyst with reflux reaction time 18 hat 135 ℃. The structure of product was confirmed by ESI-MS.

Key words:  carbon tetrachloride; phenol; aurin; synthesis

 

苯菌酮的合成工艺

叶昌伦*1何冀川2

1.四川化工职业技术学院制药与环境工程系,四川泸州646005

2. 绵阳师范学院化学与化学工程学院,四川绵阳621000

摘要:以2-甲氧基-6-甲基苯甲酸和3,4,5-三甲氧基甲苯为原料,经过溴化反应、酰氯化反应和傅克反应制备得到苯菌酮。通过对单元反应的条件优化,确认了最佳合成工艺:溴化反应中,以二氯乙烷为最佳反应溶剂,催化剂干燥铁粉最佳用量为14.3 mmol;酰氯化反应中,磺酰氯为最佳的氯化试剂;傅克反应中,最佳催化剂为四氯化钛,最佳催化剂用量为2.2 mmol。3步反应总收率为77.1%,化合物结构经过1HNMR和13CNMR确证。

关键词:苯菌酮;铁粉;四氯化钛;工艺

中图分类号:TQ45        文献标识码:A          文章编号:0258-32832017

 

Synthesis of Metrafenone YE Chang-lun1HEJi-chuan2(1. Department of pharmaceutical and environmental engineering, Sichuan Vocational College of Chemical Industry, Luzhou China; 646005; 2. School of Chemistry and chemical engineering, Mianyang Normal University, Mianyang 621000

Abstract: 2-Methoxy-6-methylbenzoic acid and 3,4,5-trimethoxytoluene were used as raw materials to prepare benzenone by bromination, acyl chlorination and Foucault reaction. The optimum reaction conditions were determined by optimizing the conditions of the unit reaction. In the bromination reaction, dichloroethane was used as the optimum reaction solvent, and the optimum amount of catalyst dry iron powdewas 14.3 mmol. The optimum chlorination reagent sulfonyl chloridewas used in the acid chlorination reaction. Titanium tetrachloride was the best catalyst and the best catalyst dosage is 2.2 mmol in the Foucault reaction. The total yield of the 3-step reaction was 77.1%, and the structure of the compound was confirmed by 1HNMR and 13CNMR.

Key words:metrafenone; iron powder; titanium tetrachloride; process

 

降血脂药瑞舒伐他汀钙重要中间体的合成工艺研究

张立光*,杨税,刘雪梅,沈亚楠,臧雪,黄倩倩

(苏州卫生职业技术学院,江苏 苏州  215009)

摘要:以对氟苯甲醛、异丁酰乙酸甲酯为原料,经环合后,用过硫酸钾氧化脱氢,再经亲核取代、还原得到瑞舒伐他汀钙重要中间体­4-(4-氟苯基)-6-异丙基-2-[(N-甲基-N-甲磺酰)氨基]嘧啶-5-甲醇,总收率为79.5%。该工艺原料价廉易得、操作简单、后处理容易、副产物较少。

关键词:4-(4-氟苯基)-6-异丙基-2-[(N-甲基-N-甲磺酰)氨基]嘧啶-5-甲醇;瑞舒伐他汀钙;合成

中图分类号:R914.5                文献标识码:A             文章编号:0258-3283(2017)

 

Synthesis of an Important Intermediate of Rosuvastatin Calcium ZHANG Li-guang*, YANG Shui, LIU Xue-mei, SHEN Ya-nan, ZANG Xue, HUANG Qian-qian(Suzhou Vocational Health College , Suzhou 215009, China), Huaxue Shiji, 2017, 39(12)

Abstract: N-(4-(4-Fluorophenyl)-5-(hydroxymethyl)-6-isopropylpyrimidin-2-yl)-N-methylmethanesulfonamide is the important intermediate compound of Rosuvastatin calcium. It was synthesized with 4-fluorobenzaldehyde and methyl 4-methyl-3-oxopentanoate as raw material, through cyclization, oxidation with potassium persulfate, nucleophilic and cyclization. The target product was synthesized in overall yield of 79.5%. The method of preparation is performed with cheap raw materials, simple operation, fewer steps and fewer by-products.

Key wordsN-(4-(4-fluorophenyl)-5-(hydroxymethyl)-6-isopropylpyrimidin-2-yl)-N-methylmethanesulfonamide; Rosuvastatin calcium; synthesis