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《化学试剂》2017年第11期中英文摘要

介孔TiO2中空微球的制备及其光催化性能研究

石凯,李巧玲*

(中北大学 理学院,山西 太原  030051

 

摘要:采用双模板辅助,经水热条件下制备出TiO2@C复合微球,高温煅烧除去模板得到介孔TiO2中空微球。利用XRDSEMTEM和氮气吸脱-脱附仪对所制备样品的晶体结构、形貌及孔结构进行表征。所制备的介孔TiO2中空微球属于锐钛矿型,是由大量直径为15.31 nm的介孔初级微球堆积而成,整体微球直径约为360 nm,加入葡萄糖作为模板剂能使孔道结构变得有序。以罗丹明B为模拟污染物,探讨了介孔TiO2中空微球光催化降解罗丹明B的性能。结果表明,在20 W紫外光照射下,50 mg介孔TiO2中空微球在30 min内可使初始浓度为10 mg/L的罗丹明B完全降解,重复使用11次,在50 min时的降解率仍可达89.5%

关键词:二氧化钛;模板法;介孔;光催化性能;罗丹明B

中图分类号:O641.2         文献标识码:A         文章编号:0258-32832017

 

Preparation and Photocatalytic Properties of Mesoporous Hollow TiO2 Microspheres SHI Kai, LI Qiao-ling*(School of science, North University of China, Taiyuan 030051 )

Abstract:TiO2 mesoporous hollow microspheres (MHMs) were prepared by double-template method viacalcinatingpercussive TiO2@C spherical composites that were hydrothermally prepared. As-obtained products were characterized XRD, SEM, TEM, and nitrogen adsorption-desorption apparatus to reveal the crystal structure and morphology. Results showed that the TiO2 MHMs are in anatase phase, constructed by large amount of mesoporous primary microspheres whose diameter is 15.31 nm. The overall diameter of TiO2 MHMs is about 360 nm. Adding glucoses as template can result in ordered pore structure. Photocatalytic degradation of Rhodamine B was conveyed as the probe reaction to evaluate the photocatalytic activity of TiO2 MHMs. Results showed that Rhodamine B (10 mg/L) could be completely degraded in 30 min under ultraviolet light irradiation (20 W) using 50 mg mesoporous hollow TiO2 microspheres. As-made TiO2 MHMs can be recyclable, the degradation rate still reached 89.5% at the 11th use.

Key words:titania;template method;mesoporous; photocatalytic properties;Rhodamine B


Pd/CNTs金属纳米催化剂的制备及其催化对氯硝基苯加氢性能

张瀚1, 2王磊2胡广林1熊春荣1尹宏峰*2

1.海南大学 材料与化工学院,海南 海口  5702282.中国科学院 宁波材料技术与工程研究所,浙江 宁波  315201

 

摘要:通过硝酸浸渍法对碳纳米管(CNTs)进行预处理改性,并采用乙二醇液相还原法制备Pd/CNTs纳米催化剂,通过XRD、TEM、BET、Raman spectra、ICP等手段对其进行了表征。结果表明,Pd/CNTs催化剂中Pd的负载量为0.9%,Pd纳米颗粒均匀地分散在CNTs表面,粒径平均大小为5 nm。该催化剂用于对氯硝基苯的选择加氢反应,在常压、60 ℃下反应2 h,该反应转化率为94.7%,选择性为89.2%。

关键词:碳纳米管;钯;对氯硝基苯;选择加氢;对氯苯胺

中图分类号O643.36       文献标识码:A             文章编号:0258-3283(2017)

 

Preparation of Pt /CNTs Nano-catalyst and Performance in Hydrogenation of p- Chloronitrobenzene ZHANG Han1,2 , WANG Lei2, HU Guang-lin1, XIONG Chun-rong1, YIN Hong-feng*2(1.College of Materials and Chemical Engineering, Hainan University, Haikou 570228, China; 2. Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China)

Abstract:Pd/CNTs nanocatalyst was prepared by pretreatment of carbon nanotubes (CNTs) followed with liquid phase reduction method. The catalyst was characterized by XRD, TEM, BET, Raman spectra and ICP. The results showed that the loading of palladium on Pd/CNTs catalyst was 0.9%, palladium nanoparticles highly dispersed on the surface of CNTs with average diameter of 5 nm. The catalyst was used for selective hydrogenation of chloronitrobenzene and the hydrogenation conversion was 94.7% and the selectivity was 89.2%.

Key wordsnanotubes; palladium; chloronitrobenzene; selective hydrogenation; chloroaniline

 

 

2-芳醛腙噻唑类化合物的合成及其抗肿瘤活性

李韦韦,姚敏娜,卜伟,王婧雯,文爱东*

(第四军医大学第一附属医院 药剂科,陕西 西安  710032)

 

摘要:噻唑环和腙键结构均具有一定的生物活性,采用活性结构拼接法,将噻唑环与腙键相结合,设计并合成了16个2-芳醛腙噻唑类化合物,并采用MTT法对目标化合物进行体外抗肿瘤活性筛选。测试结果表明,该类新化合物对乳腺癌细胞细胞系(MDA-MB-231、MDA-MB-468、MCF-7)具有一定的抗增殖活性。其中,N-(2-吡啶)甲醛-2-(4-苯基)噻唑腙的抗增殖活性最好,其IC50值分别为(0.21± 0.11)、(0.18 ± 0.10)、(0.17 ± 0.08)μmol/L;而该化合物对其他肿瘤细胞亦具有一定的抗增殖活性,且相对乳腺癌细胞株的生物活性均在10倍及以上,说明其对乳腺癌细胞具有较好的生物活性和选择性,且毒副作用小,值得作为抗乳腺癌先导化合物进行进一步研究。

关键词噻唑环;腙键;乳腺癌细胞;抗增殖活性;选择性

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

 

Synthesis and Antitumor Activity of 2-Thiazolylhydrazyne Scaffold Derivatives LI Wei-wei, YAO Min-na, BU Wei, WANG Jing-wen, WEN Ai-dong* (Department of Pharmacy, Xijing Hospital, Fourth Military Medical University, Xi’an 710032, China)

Abstract:Thiazole ring and hydrazone structure have certain biological activity. In this work, we applied the active structure-linking method, which is combining thiazole and hydrazone, and have designed and synthesized a series of novel 2-thiazolylhydrazyne scaffold derivatives.The structures were confirmed by 1HNMR and elemental analysis. These compounds were evaluated for anti-breast cancer activity on MDA-MB-231, MDA-MB-468, MCF-7 cells by MTT method in vitro. The test results show that this kind of new compounds has antiproliferative activity. And N-(4-phenyl-thiazole- 2-yl)-2-pyridine hydrazone exhibited better antiproliferative activity against MDA-MB-231, MDA-MB-468, MCF-7breast cells with the IC50 value of 0.21±0.11、0.18±0.10、0.17±0.08 μmol/L, respectively.This compound also has certain antiproliferative activity against the other tumor cells (PANC-1, Hela, MKN45, SKOV3, Karpas299, Ramos). And the relate selectivity of compound against MDA-MB-231 cell are more than 10 times. The results show that it has good biological activity and selectivity against breast cancer cells with low side effects. So above compound is worth as lead compound of breast cancer for further research.

Key words:thiazole; hydrazone; breast cancer cells; antiproliferative activity; selectivity

 


2-芳醛腙噻唑类化合物的合成及其抗肿瘤活性

李韦韦,姚敏娜,卜伟,王婧雯,文爱东*

(第四军医大学第一附属医院 药剂科,陕西 西安  710032)

 

摘要:噻唑环和腙键结构均具有一定的生物活性,采用活性结构拼接法,将噻唑环与腙键相结合,设计并合成了16个2-芳醛腙噻唑类化合物,并采用MTT法对目标化合物进行体外抗肿瘤活性筛选。测试结果表明,该类新化合物对乳腺癌细胞细胞系(MDA-MB-231、MDA-MB-468、MCF-7)具有一定的抗增殖活性。其中,N-(2-吡啶)甲醛-2-(4-苯基)噻唑腙的抗增殖活性最好,其IC50值分别为(0.21± 0.11)、(0.18 ± 0.10)、(0.17 ± 0.08)μmol/L;而该化合物对其他肿瘤细胞亦具有一定的抗增殖活性,且相对乳腺癌细胞株的生物活性均在10倍及以上,说明其对乳腺癌细胞具有较好的生物活性和选择性,且毒副作用小,值得作为抗乳腺癌先导化合物进行进一步研究。

关键词噻唑环;腙键;乳腺癌细胞;抗增殖活性;选择性

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

 

Synthesis and Antitumor Activity of 2-Thiazolylhydrazyne Scaffold Derivatives LI Wei-wei, YAO Min-na, BU Wei, WANG Jing-wen, WEN Ai-dong* (Department of Pharmacy, Xijing Hospital, Fourth Military Medical University, Xi’an 710032, China)

Abstract:Thiazole ring and hydrazone structure have certain biological activity. In this work, we applied the active structure-linking method, which is combining thiazole and hydrazone, and have designed and synthesized a series of novel 2-thiazolylhydrazyne scaffold derivatives.The structures were confirmed by 1HNMR and elemental analysis. These compounds were evaluated for anti-breast cancer activity on MDA-MB-231, MDA-MB-468, MCF-7 cells by MTT method in vitro. The test results show that this kind of new compounds has antiproliferative activity. And N-(4-phenyl-thiazole- 2-yl)-2-pyridine hydrazone exhibited better antiproliferative activity against MDA-MB-231, MDA-MB-468, MCF-7breast cells with the IC50 value of 0.21±0.11、0.18±0.10、0.17±0.08 μmol/L, respectively.This compound also has certain antiproliferative activity against the other tumor cells (PANC-1, Hela, MKN45, SKOV3, Karpas299, Ramos). And the relate selectivity of compound against MDA-MB-231 cell are more than 10 times. The results show that it has good biological activity and selectivity against breast cancer cells with low side effects. So above compound is worth as lead compound of breast cancer for further research.

Key words:thiazole; hydrazone; breast cancer cells; antiproliferative activity; selectivity

 

 

 

新型复合材料MnFe2O4@SiO2-NH2的制备

及其固定青霉素G酰化酶

杜传虎,薛屏*,谷耀华,胡春苗

(宁夏大学能源化工重点实验室,宁夏银川 750021

 

摘要:通过溶剂热法制备出高磁性的聚合物微球MnFe2O4,经正硅酸乙酯(TEOS)和3-氨基丙基三乙氧基硅烷(APTS)对微球表面进行改性修饰,制备出新型复合材料MnFe2O4@SiO2-NH2,并将其用于固定化青霉素G酰化酶。在Si/Fe比为7 mmol/g、n(TEOS): n(APTS) = 1:1时,固定化酶PGA/MnFe2O4@SiO2-NH2在37℃下水解青霉素G钾合成6-氨基青霉烷酸,表观酶活为1660 IU/g、载酶量为107.1 mg/g、比活性为15.5 IU/mg、活性回收率为46.9%。经过6次重复使用,保留初始酶活的81.3%,在使用中固定化酶在磁场的作用下能够快速沉降与产物分离。

关键词:磁性复合材料;固定化青霉素G酰化酶;催化活性

中图分类号:O643                文献标识码:A                文章编号:0258-32832017

 

Preparation of New Composite MnFe2O4@SiO2-NH2 and Immobilization for Penicillin G AcylaseDUChuan-hu,XUE Ping*, GU Yao-hua, HU Chun-miao(Key Laboratory of Energy Resources &Chemical Engineering , Ningxia University , Yinchuan 750021, China)

Abstract: High magnetic polymer microspheres MnFe2O4 were prepared by solvothermal method.Themagnetic composite materials MnFe2O4@SiO2-NH2were prepared by using tetraethoxysilane (TEOS) and 3-aminopropyl triethoxysilane (APTS) to decorating the surface of the microspheres MnFe2O4, and were used as the support for immobilization of penicillin G acylase (PGA).When the Si/Fe was 7 mmol/g and n(TEOS) :n(APTS ) = 1:1,the apparent activity of PGA/MnFe2O4@SiO2-NH2for hydrolyzing penicillin G potassium into6-aminopenicillanic acid at 37℃was 1660 IU/g, the enzyme load was about 107.1 mg/g, the specific activity was 15.5 IU/mg, and the activity recovery was about 46.9% and retained the initial activity of 81.3% after 6 recycles.The PGA/MnFe2O4@SiO2-NH2 can settle quickly in the magnetic field and be separated easily from the product in applications.

Key words:magnetic composite materials; immobilized penicillin G acylase; catalytic activity

 


去甲去氢斑蝥素酰亚胺衍生物的合成及抑菌活性

曾造*,李金海,舒群威,吕敬松

(贵州工程应用技术学院 化学工程学院 贵州省应用化学特色重点实验室,贵州 毕节 551700

 

摘要:以顺丁烯二酸酐和呋喃为起始原料,经Diels-Alder、取代和缩合反应,合成了7个去甲去氢斑蝥素酰亚胺衍生物,其结构经NMR和元素分析证实。通过滤纸片法,分别测定合成物对大肠杆菌、金黄色葡萄球菌的抑菌活性。结果表明,中间体N-氨基去甲去氢斑蝥素酰亚胺和部分产物对两种细菌都有较好的抑菌活性。其中,N-(氨基缩对甲氧基苯甲醛)-去甲去氢斑蝥素酰亚胺对大肠杆菌的抑菌活性最强,抑菌圈直径为28 mm。

关键词:去甲去氢斑蝥素;酰亚胺衍生物;合成;抑菌活性

中图分类号: O625.6         文献标识码A       文章编号:

 

Synthesis and Bacteriostatic Activity of Dehydronorcantharidin Imide Derivatives ZENG Zao *, LI Jin-hai, SHU Qun-wei, LV Jing-song (Guizhou Key Laboratory of Applied Chemistry, School of Chemical Engineering, Guizhou University of Engineering Science, Bijie 551700, China)

Abstract: In this work, seven dehydronorcantharidin imide derivatives were synthesized through Diels-Alder,substitution and condensation from furan and maleic anhydride.The structures of synthetic compounds were confirmed by NMR and elemental analysis. The bacteriostatic activity of synthetic compounds against Escherichia coli and Staphylococcus aureus were tested by the method of filter-paper. The result shown that the N-amino dehydronorcantharidin and some compounds against two bacteria had obvious antibacterial activity. Especially, N- amino- 4-methoxybenzaldehyde dehydronorcantharidin against Escherichia coli was the best,and the inhibition zone diameter was 28 mm.

Key words: dehydronorcantharidin; imide derivatives; synthesis; bacteriostatic activity

 


反相微乳法制备DMCC用于催化二氧化碳与环氧丙烷共聚

周钰1, 2,唐喆1,许琦*1

(1.  盐城工学院化学化工学院,江苏盐城2240512.常州大学石油化工学院,江苏常州  213164)

 

摘要:通过反相微乳法和共沉淀法合成了钴锌双金属氰化物催化剂。研究了制备方式及共聚反应条件对其催化性能及聚碳酸酯组成的影响。结果表明,反相微乳法制备的DMCC-1具有较低的结晶度且可以络合更多的有机配体,且在80℃、4MPa的条件下,采用一步加料法催化CO2与环氧丙烷共聚所制备的聚碳酸酯中碳酸酯单元量达43.5%,数均分子量达36400,且聚合物分散指数仅为2.07。共聚结果表明一步加料法有利于提高聚合物的数均分子量,而逐步加料法有利于降低聚合物的相对分子量分布。

关键词:双金属氰化物催化剂;反相微乳法;二氧化碳;环氧丙烷;聚碳酸酯

中图分类号:O643.32文献标识码:A      文章编号:0258-32832017

 

DMCC Prepared via Reverse MicroemulsionMethod and Catalytzed Copolymerization of Carbon Dioxide withPropylene Oxide ZHOU Yu1,2,TANG Zhe1, XU Qi*1(1. School of Chemistry and Chemical Engineering, Yancheng Institute of Technology, Yancheng 224051, China;2. College of Chemistry and Chemical Engineering, Changzhou University, Changzhou 213164, China)

Abstract:Cobalt zinc double metal cyanide catalysts were prepared by reverse micro emulsion method and coprecipitation method. The effect of preparation and reaction condition on catalytic performance and the polycarbonate composition were investigated. The results revealed that DMCC-1 prepared by reverse microemulsion method had lower crystallinity and complexed more organic ligand. The polycarbonate synthesized from CO2 and propylene oxide in the presence of DMCC-1 under the conditions of 80 °C,4 MPaandone-step feed modepossessed the molar fraction of carbonate linkages in the produced polymer was43.5%,number average molecular mass up to 36400 and polydispersity index was 2.07.At the same time, it was found that theone-step feed mode could improve the number average molecular of the polycarbonate, but interval feed mode could reduce thepolydispersity index of the polycarbonate.

Keywords: double metal cyanide catalyst; reverse microemulsionmethod; carbon dioxide; propylene oxide; polycarbonate

 

6-(呋喃-2-亚甲氨基)-2-甲基-1H-吲哚-3-羧酸乙酯的合成、表征与生物活性研究

画莉1,万茂生*1,童张法2,陈丹1,李传宗1,苏月清1

(1.  贺州学院 材料与环境工程学院,广西 贺州  542899

(2.  广西大学 化学化工学院,广西 南宁  530004

 

摘要:以2, 4-二硝基氯苯为原料,经过3步反应得到标题化合物。当温度为78 ℃,反应时间为8.5 h,目标化合物的收率可达65%。通过IR、1HNMR、13CNMR和MS光谱技术对其结构进行表征。运用SRB法评价了目标化合物对人体肺癌细胞生长抑制活性。初步的生物实验表明,该化合物对癌细胞H1792,A549,H157和Calu-1具有生长抑制作用,且具有浓度依赖性。细胞周期分析发现其能诱导Calu-1细胞凋亡。

关键词:6-(呋喃-2-亚甲氨基)-2-甲基-1H-吲哚-3-羧酸乙酯;合成;表征;生物活性

中图分类号: O626.1               文献标识码: A             文章编号:0258-32832017

 

Synthesis, Characterization and Biological Activity of Ethyl 6-(Furan-2-ylmethyleneamino)-2-Methyl-1H-Indole-3-Carboxylate HUA Li1, WAN Mao-sheng*1, TONG Zhang-fa2, CHEN Dan1LI Chuan-zong1, SU Yue-qing1(1.College of Material and Environmental Engineering, Hezhou University, Hezhou 542899, China; 2. School of Chemistry& Chemical Engineering, Guangxi University, Nanning 530004, China), Huaxue Shiji, 2017, 39(10)

Abstract:Ethyl 6-(furan-2-ylmethyleneamino)-2-methyl-1H-indole-3-carboxylate was synthesized via three-step reaction using 2, 4-dinitrochlorobenzene as the material. When the reaction temperature was 78℃ and reaction time was 8.5 h, the yield of target compound by the column chromatography reached 65%. The structure of compound was confirmed by IR, 1HNMR, 13CNMR and MS. Growth inhibitory activity of 6-(furan-2-ylmethyleneamino)-2-methyl-1H-indole-3-carboxylate on human lung cancer cells was evaluated by the method of SRB. The preliminary biological experiments showed that compound possessed growth inhibition activity to cancer cells H1792, A549, H157 and Calu-1 in a dosage dependent manner. It was found that compound induced apoptosis of Calu-1 cells by cell cycle analysis.

Key wordsEthyl 6-(furan-2-ylmethyleneamino)-2-methyl-1H-indole-3-carboxylate; synthesis; characterization; biological activity

 

 

 

化学计量银促进的偶联反应研究进展

季玉雯,秦晓露,殷晓婷,胡静伟,王晨,程凯*

(绍兴文理学院 化学化工学院,浙江 绍兴   312000)

 

摘要:过渡金属银由于其催化反应符合绿色化学的原则,在有机合成中的应用成为近年来研究的热点。但实际上化学计量的银往往被作为助剂以提高金属离子的反应活性,而银化合物本身作为催化剂的应用却十分有限。针对此类问题,近年来的工作集中在利用银配合物的σ-和π-路易斯酸性性质研究银催化的反应。综述了银促进的偶联反应在C-P(N、S)键的形成和三氟甲基化反应研究中的应用和进展。

关键词银促进;偶联反应;C-P(N、S)键的构筑;三氟甲基化反应

中图分类号:O621. 3            文献标识码:A           文章编号:0258-3283(2017)

 

Research Progress in Equivalent Ag-Mediated Coupling Reactions JI Yu-wen, QIN Xiao-lu, YIN Xiao-ting, HU Jing-wei, WANG Chen, CHENG Kai * (College of Chemistry and Chemical Engineering,Shaoxing University,Shaoxing 312000,China) Huaxue Shiji,2017,39

AbstractThe application of transition metal silver in organic synthesis has been a hot topic in recent years because of its catalytic reaction to the principle of green chemistry. But in fact, the silver of stoichiometry is often used as an auxiliary agent to improve the reaction activity of metal ions while the use of silver compounds as catalysts is very limited. In response to such problems, the work in recent years has focused on the study of silver catalytic reactions using the sigma - and pi-lewis acid properties of the silver complex. Equivalent Ag-mediated coupling reactions has been widely studied in organic synthesis. The research progress on Ag-mediated cross-coupling is reviewed, focusing on applications and progress of the construction of C-P(N, S) bonds and trifluoromethylation.

Key wordsAg-mediated; coupling reaction; construction of C-P(N, S) bonds; trifluoromethylation

 

 

分子印迹固相萃取技术在食品安全检测中的应用进展

田春霞

(北京有色金属研究总院,北京100088

 

摘要:分子印迹固相萃取技术(MISPE)是一种高效的样品前处理技术,能从复杂的样品中选择性分离目标物及其结构类似物。分子印迹技术( MIT) 在食品中农药和兽药残留检测中的应用快速发展。综述了近两年国内外分子印迹固相萃取技术在食品安全检测中农药、兽药残留检测的应用及进展,讨论了当前分子印迹固相萃取技术在食品安全检测应用中存在的问题,并对其发展趋势进行了展望。

关键词:分子印迹固相萃取技术(MISPE);食品安全;农药和兽药残留;应用进展

中图分类号O658            文献标识码:A             文章编号:0258-32832017

 

Application Developmentof Molecularly Imprinted Solid-phase Extraction Technologyon Detection in Food Safety TIAN Chun-xia (Beijing General Research Institute for Nonferrous Metals, Beijing 100088)

Abstract: Molecularly imprinted solid-phase extraction technology (MISPE) is a sample pretreatment technology with high performance, which can separate target molecules and structurally similar molecules from complex samples selectively. Applications of molecular imprinted technology ( MIT) on detection of pesticide residues and veterinary drugs residues in food have been developed rapidly. This paper reviews application development of molecularly imprinted solid-phase extraction technology on detection in food safety in recent two years. Besides, the current problems and the future development of the technology are discussed.

Key words: molecularly imprinted solid-phase extraction(MISPE); food safety; pesticides residues and veterinary drugs residues; application development

 

金属配合物抗癌活性的研究进展

                          吴月红

(吉林工程职业学院  粮食与食品工程学院,吉林 四平  136000

 

摘要:自从发现顺铂具有抗癌活性以来,金属配合物作为新一类抗癌药物引起了人们的广泛关注。综述了近年来铂类配合物、钌类配合物和席夫碱配合物在抗癌药物中的研究进展,重点阐述了铂类配合物抗癌活性的研究现状及作用原理,并对金属配合物抗癌活性的研究进展进行总结,为金属配合物抗癌药物研究提供参考和依据。

关键词:金属配合物;抗癌活性;铂类配合物;钌类配合物

中图分类号:O641.4                文献标识码:A                文章编号:0258-32832017

 

Progress in Anticancer Activity of Metal Complexes WU Yue-hong (         , Jilin Engineering Vocational College, Siping 136000, China), Huaxue Shiji, 2017, 39(10)

Abstract: Since the discovery of the anticancer activity of cisplatin, as a new class of anticancer drugs, metal complexes have attracted extensive attention. Recent advances in the researches on platinum complexes, ruthenium complexes and Schiff bases in anticancer drugs are reviewed. The research status and principle of the anticancer activity of platinum complexes are emphasized. And the research progress of the anticancer activity of metal complexes is summarized. It provides reference and basis for the new research field of anticancer drugs of metal complexes.

Key words: metal complexes; anticancer activity; platinum complexes; ruthenium complexes

 


高效液相色谱-串联质谱法测定粮谷中十二环吗啉和十三吗啉残留量

 

曹海微1,田芳洁2,康明芹1*,李荣荣1,杨璐1,顾婷婷1

1. 吉林出入境检验检疫局,吉林 长春 130062

   2. 长春市食品药品监督管理局南关监督管理所,吉林 长春 130062

 

摘要:建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定粮谷中十二环吗啉和十三吗啉残留量的分析方法。样品经1%甲酸-乙腈超声提取,石墨化炭黑/氨基复合固相萃取柱净化,HPLC-MS/MS多反应监测模式测定,外标法定量。结果表明,十二环吗啉和十三吗啉在2.0 ~ 200.0 µg/L范围内线性关系良好,相关系数均大于0.999。本方法十二环吗啉和十三吗啉的定量限分别为2.0 μg/kg和5.0 μg/kg,样品基质中两种目标物在3个添加水平的平均回收率为78.0 % ~ 96.0 %,相对标准偏差(RSD)为3.0 % ~ 8.2 %。该方法简单、灵敏、准确、可靠,可用于粮谷中十二环吗啉和十三吗啉残留分析。

关键词:高效液相色谱-串联质谱;粮谷;十二环吗啉;十三吗啉

中图分类号:O657.63      文献标识码:A    文章编号:0258-32832017

 

Determination of Dodemorph and Tridemorph in Grain using High Performance Liquid Chromatography-tandem Mass Spectrometry CAO Hai-wei, TIAN Fang-jie, KANG Ming-qin*, LI Rong-rong, YANG lu, GU Ting-ting1. Quarantine Technology Center of Jilin Entry-Exit Inspection and Quarantine Bureau, Changchun 130062; 2. Nanguan Supervision Institute of Changchun food and Drug Administration Inspection, Changchun 130062

Abstract: High performance liquid chromatography-trandem mass spectrometry(HPLC-MS/MS) was applied to determine the dodemorph and tridemorph residues in grain.The analytes in samples were extracted using 0.1 % formic acid - acetonitrile mixture as the extraction solvent and were further purified with the ENVI-Carb/LC cartridge. The purified liquid was detected using HPLC-MS/MS and quantified using external standard method. The results showed that the good linear range for dodemorph and tridemorph were 2.0 ~ 200. 0 μg/L, and the correlation coefficients were higher than 0. 999. The limit of quantification for the dodemorph and tridemorph was 2.0 μg/kg and 5.0 μg/kg respectively. The recoveries of the analytes at three spiked levels ranged between 78.0 % and 96.0 % with the relative standard deviations of 3.0 % ~ 8.2 %. The present method is simple, sensitive, reliable and accurate which can be suitible for dodemorph and tridemorph analysis of grain.

Key words: HPLC-MS/MS; grain; dodemorph; tridemorph

 

 

 

异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物

 

方诚,凌芳*,郑琦,陈浩云

(国药集团化学试剂有限公司,上海200002

 

摘要:本文通过从样品成分特点和测试原理入手,对异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物的影响因素作了初步分析和讨论。其中对实验过程中样品取样量、显色体系pH、显色温度、显色反应时间及氧化剂的选择进行了优化。测试结果显示,本方法的最佳取样量为0.1g,最佳显色温度为35℃,最佳反应时间为40 min,线性回归方程Y=0.0025+2.1168 X,方法检出限为0.0014 μg/mL。该研究为今后硫酸铵中氰化物的测定提供了一定的技术支撑。

关键词:硫酸铵;异烟酸-吡唑啉酮光度法;氰化物

中图分类号:O623.76      文献标识码:A     文章编号:

 

IsonicotinicAcid – pyrazoloneSpectrophotometric Determination of Cyanide in Ammonium Sulfate FANG Cheng, LING Fang*, ZHENG QiCHEN Hao-yunSinopharm Chemical Reagent Co., LTD , Shanghai200002

AbstractIn this paper, the factors affecting the determination of cyanide in ammonium sulfate are analyzed and discussed starting with the composition, characteristics and testing principle of the sample. The sample size, color rendering system, pH, color rendering temperature, color reaction time and oxidant selection were optimized.The results show the optimum sampling weights was 0.1g,the optimum temperature was 35℃ and the optimum time was 40 min. The linear equation is Y=0.0025+2.1168X.The detection limit was 0.0014μg/mL.The cyanide in ammonium sulfate was determined by isonicotinicacid-pyrazolonespectrophotometry.

Keywords:ammonium sulfate; isonicotinic acid -pyrazolone spectrophotometric method ;cyanide

 

马兰头及其产地环境主要污染物现状评价

蔡志平1,朱杰丽*2,杨柳 2,蒋步云2,吴翠蓉2,蔡铃潇3,黄莎3

1. 缙云县括苍山林场,浙江 缙云  3214002. 浙江省林产品质量检测站,浙江 杭州  3100233. 临安市林业局,浙江 临安  311300

 

摘要:通过对浙江省马兰头及其土壤中5种重金属和12种农药分析与污染评价,为马兰头及其产地环境的质量安全评价提供科学依据。对浙江省马兰头样品中铅、镉、铬元素含量采用湿法消解,砷、汞元素含量采用微波消解,12种农药分别采用气相色谱仪和液相色谱仪进行测定,并与相关标准进行比对和评价。结果表明,马兰头及其产地中拟除虫菊酯均有不同程度地检出且存在超标现象。从综合污染指数来看,浙江省马兰头受污染较轻,品质基本安全;研究区域内马兰头中PbCdCrAsHg5种重金属平均含量为0.180.0731.10.0460.004 mg/kg,其平均含量分别达到了标准限量的180%146%220%23%40%;研究区域内产地环境中5种重金属含量大致顺序为Cr > Pb > As> Hg > CdC.V26.4% 278%之间,表现出极大的非均匀性,表明不同种类重金属元素之间存在很大差异性。综合污染指数,除1个采摘点已达到重污染水平,其他3个采样点均未受到污染,处于清洁水平。

关键词:野菜;土壤;污染物;评价;浙江省

中图分类号:S667.6      文献标识码:A      文章编号:0258-32832017

 

Investigation and Assessment of Heavymetal Contentand Pesticide Residuein Indian Kalimeris Herb and Soils

AbstractIn order to provide scientific basis for the quality and safety assessment in Indian Kalimerisherb and soils, the pollution levels of 5 heavy metals and 12 pesticides have been investigated.The content of Pb, Cr and Cd was determined by using wet digestion. The content of As and Hg was determined by using microwave digestion and the content of pesticide was determined by using Agilent7890 gas chromatography and Dionex P680 liquid chromatography. And the content were compared and evaluated with the relevant standards. The results showed that:Synthetic pyrethroids pesticides were detectable and some has exceeded the tolerance of nationalstandards. From the integrated pollution index, Indian Kalimerisherb were not polluted by pesticides. The average concentration of Pb、Cd、Cr、As、Hg was 0.18、0.073、1.1、0.046、0.004 mg/kg respectively.The ratio of concentration and criterion of five elements in edible wild potherb was Pb(180%)、Cd(146%),Cr(220%)、As(23%)、Hg(40%) respectively. The order of the average concentration of Pb、Cd、Cr、As、Hg in soil was Cr >Pb> As> Hg > Cd, the range of variation coefficient was from26.4% to 278%. The results showed great heterogeneity, which indicates that there is a big difference between different kinds of heavy metal elements. The comprehensive pollution indexes of the soil heavy metals were all smaller than1 except for one soil picking point (3.89).

Key Wordsedible wild potherb;soil;pollutants;evaluation,Zhejiang province

 

 

 

 

可见光下离子液体-TiO2体系降解甲基橙废水研究

郭加武辛炳炜*赵旋徐瑞华孙梦晓

(德州学院 山东高校配位化学与功能材料重点实验室,山东 德州  253023)

 

摘要:将离子液体[bmim]X (X= Br、PF6、Tf2N)和TiO2 P25纳米颗粒物理掺杂,构建[bmim]X-TiO2光催化混合体系,利用可见光照射实现了甲基橙废液的降解。探讨了离子液体的用量、可见光照射时间、阴离子种类等因素发现,[bmim]Br-TiO2 P25(物质的量比为20︰1)80 min可将10.0 mg/L甲基橙溶液完全脱色,[bmim](CF3SO2)2N-TiO2 P25(物质的量比为20︰1)仅需60 min,而单纯的TiO2 需要160 min。实验结果表明,离子液体可促使TiO2在可见光下很好地完成甲基橙的降解脱色。

关键词:离子液体;二氧化钛;可见光;甲基橙

中图分类号:O643.3      文献标识码:A        文章编号0258-3283(2017)

 

Photocatalytic Performance of Ionic Liquid-TiO2 Mixture to Methyl Orange Waste Water Under Visible Light GUO Jia-wu, XIN Bing-wei*, Zhao Xuan, XU Rui-hua, SUN Meng-xiao(Key Laboratory of Coordination Chemistry and Functional Materials in Universities of Shandong, Dezhou University, Dezhou 253023, China), Huaxue Shiji, 2017, 39(10)

Abstract: Ionic liquid-TiO2mixing system was constructed by physically mixing ionic liquid and TiO2 P25. The catalytic system [bmim]Br-TiO2 P25 with mole ratio of 20︰1 could degrade 10.0 mg/L methyl orange to almost colourless after being illuminated by visible light for 80 min, while [bmim](CF3SO2)2N-TiO2 P25 (mole ratio with 20︰1)only needed 60 min under same condition. TiO2 carried out decolorization of methyl orange in 160 min. The result suggestedthat ionic liquids could improve the catalytic activity of TiO2 under visible light.

Key words: ionic liquid; titanium dioxide; visible light; methyl orange

 


多环芳烃菲和荧蒽半抗原的制备及量化计算

刘媛媛1,陈奇娜1,潘学春2,黄江春2,李壹*2

(1. 东南大学成贤学院 制药与化学工程学院,江苏 南京  210088

2. 南京工业大学 食品与轻工学院,江苏 南京  211816)

 

摘要:以多环芳烃菲和荧蒽为原料,分别与丁二酸酐发生傅克酰基化反应,制备γ-羰基-2-菲丁酸(I)和γ-羰基-3-荧蒽丁酸(III),再经黄鸣龙还原制备半抗原2-菲丁酸(II)和3-荧蒽丁酸(IV),产品结构经熔点、IR和1HNMR表征。采用量子化学计算优化半抗原II和IV的分子构型,获得前线轨道、能量、电子分布及稳定性等信息,辅助半抗原的设计和筛选,为制备高特异性人工抗原奠定了基础。

关键词:菲丁酸;荧蒽丁酸;傅克酰基化反应;黄鸣龙还原;量子化学计算

中图分类号:O625.1        文献标识码:A             文章编号:0258-32832017

 

Phe Preparation and Quantum Chemical Calculation of Polycyclic Aromatic Hydrocarbons nanthrene and FluorantheneHaptens LIU Yuan-yuan1, PAN Xue-chun2, HUANG Jiang-chun1, LI Yi*2 (1. Department of Chemical and Pharmaceutical Engineering, Southeast University ChengXian College, Nanjing 210088, China; 2. College of Food Science and Light Industry, Nanjing Tech University, Nanjing 211816, China)

Abstract:Using polycyclic aromatic hydrocarbons phenanthrene and fluoranthene as starting materials, 4-oxo-4-(phenanthren-2-yl)butanoic acid (I) and 4-(fluoranthen-3-yl)-4-oxobutanoic acid (III) were synthesized by the Friedel-Crafts acylation with dihydrofuran-2,5-dione, respectively. Then haptens 4-(phenanthren-2-yl)butanoic acid (II) and 4-(fluoranthen-3-yl)butanoic acid (IV) were prepared via Huang Min-lon reduction. The structures were confirmed by melting point, IR and 1HNMR. The molecular configurations of haptens II and IV were optimized by quantum chemical calculation, and the frontier orbital energy, electronic distribution and stability were obtained. These parameters can assist the design and screening of hapten, and lay the foundation for the preparation of high specific antigen.

Key words4-oxo-4-(phenanthren-2-yl)butanoic acid; 4-(fluoranthen-3-yl)-4-oxobutanoic acid; Friedel-Crafts acylation; Huang Min-lon reduction; quantum chemical calculation

 

 

外源抗氧化剂7-(4-氨基-1, 2, 4-三唑-5-)硫乙氧基黄酮及其乙酰化产物的合成

段志芳*,邵玲,刘文华

(肇庆学院 生命科学学院,广东 肇庆  526061

 

摘要:7-溴乙氧基黄酮与3-取代-4-氨基-1,2,4-三唑-5-硫醇类化合物缩合反应得到7-(4-氨基-1, 2, 4-三唑-5-)硫乙氧基黄酮,为了增加其脂溶性,将该类化合物进一步与乙酸酐回流反应12 h,得到的化合物不是预期的7-(3-取代-4-乙酰氨基-1,2,4-三唑-5-)硫乙氧基黄酮衍生物,而是7-[3-取代-4-(2-乙酰氧基)-乙亚氨基-1, 2, 4-三唑-5-]硫乙氧基黄酮,分别用红外、核磁共振氢谱及碳谱、质谱和元素分析对这4个乙酰化产物的结构进行了确证。以清除超氧自由基、羟自由基、亚硝基自由基和2, 2-二苯基-1-苦味酰基自由基的活性及总还原能力为指标,比较测定了4个7-(3-取代-4-氨基-1,2,4-三唑-5-)硫乙氧基黄酮化合物及其意外乙酰化产物的体外抗氧化活性。结果表明,在测定浓度下,乙酰化衍生物7-[3-对甲氧苯基-4-(2-乙酰氧基)-乙亚氨基-1,2,4-三唑-5-]硫乙氧基黄酮较其前体抗氧化活性强。

关键词:三唑;黄酮;乙酰化;合成;抗氧化

中图分类号:O629.9     文献标识码:A      文章编号:0258-3283(2017)

 

Synthesis of 7-(4-Amino-1,2,4-triazol-5-) thioethoxy Flavones and their Acetylated Derivatives as Exogenous Antioxidants DUAN Zhi-fang, SHAO Ling, LIU Wen-hua (College of Life Science,Zhaoqing University, Zhaoqing 526061, China)

Abstract: 7-(3-Substituent-4-amino-1,2,4-triazol-5-) thioethoxy flavones were synthesized by the reaction of  3-substituent-4-amino -1,2,4-triazol-5- mercaptan and 7-bromoethoxy flavones. In order to increase the lipid solubility, continued to reacted with acetic anhydride under refluxing condition for 12 h. But the obtained products were not the corresponding acetylated derivatives 7-(3-substituent-4-acetamino-1,2,4-triazol-5-) thioethoxy flavones, they were 7-[3- substituent -4-(2- acetoxy)-ethylimino-1,2,4-triazol-5-] thioethoxy flavones. The structures of these new flavone derivatives containing triazole heterocycle were confirmed by IR, 1HNMR, 13CNMR, ESI-MS and EA. By testing the scavenging effects on the superoxide radical, hydroxyl radical, nitroso radicals, 2, 2-diphenyl-1-picryl hydrazyl free radical and total reduction activities, theantioxidative activities were compared in vitro. The results showed that at the concentration of determination, the acetylated derivative 7-[3-p- methoxyphenyl -4-(2- acetoxy)-ethylimino-1,2,4-triazol -5-]thioethoxy flavone had stronger antioxidation effects than its precursor.

Key words:triazol; flavone; acetylation; synthesis; antioxidation

 

 

 

2-吗啉醇盐酸盐的手性合成及晶体结构

田芳杰­1,肖新荣*1贾小鹏2,郭倩1,罗甜1

 (1. 南华大学 化学化工学院,湖南 衡阳  421001

2. 石药集团中央研究院,河北 石家庄  050000)

 

摘要:以单一手性纯试剂与外消旋体化合物反应,合成了4对手性纯化合物(2R, 3R, 5S)-2-吗啉醇盐酸盐及其对映体(2S, 3S, 5R)-2-吗啉醇盐酸盐。结构经IR、1HNMR、13CNMR及ESI-MS表征,利用X-射线单晶衍射法测定了其中一对对映体的空间构型。利用吗啉六元环椅式构象比船式构象稳定的特性,系统探讨以构象稳定性促进目标化合物构型形成的手性化合物合成机制及规律,为手性化合物合成方法提供新启示。

关键词手性;吗啉醇;合成;晶体结构

中图分类号:TQ460.1             文献标识码:A             文章编号:0258-32832017

 

Synthesis and Crystal Structure of Chiral 2-MorpholinolHydrochloride Tian Fang-jie1 , Xiao Xin-rong*1, Jia Xiao-peng2, Guo Qian1, Luo Tian1 (1. School of Chemistry and Chemical Engineering, University of South China, Hengyang, Hunan 421001, China; 2. Shijiazhuang Pharmaceutical Group co., ltd, AcademiaSinica, Shijiazhuang, Hebei, 050000, China)

Abstract: Four pairs of chiral compounds (2R, 3R, 5S) -2- morpholinol hydrochloride and their enantiomers (2S, 3S, 5R)-2-morpholinol hydrochloride were synthesized by the chiral reagents with raceme compounds. The structures were confirmed by IR, 1 HNMR, 13CNMR and ESI-MS. The crystal structures of enantiomer were determined by X-ray single-crystal diffraction analysis The mechanism and regularity of the synthesis of chiral morpholinol compounds were investigated by means of the higher stability of chair conformation that of boat conformation, which facilitate the formation of target compound steric configuration. This provides a new enlightenment for the study ofthe synthesis of chiral compounds

Key words:chiral; morpholinol; synthesis; crystal structure

 

 

罗丹明类荧光探针的合成及其对Hg2+的识别研究

肖潜*

(韩山师范学院 化学与环境工程学院, 广东 潮州  521041

 

摘要:以罗丹明B、水合肼及2’-羟基苯乙酮等廉价化合物为原料,经过简单的缩合反应得到可识别Hg2+的荧光探针L,其结构经1HNMR13CNMR以及HR-MS表征。光谱性能研究表明,探针LEtOH-H2O (V (EtOH): V(H2O) = 4 : 1pH 7.020 mmol/L HEPES)体系中,对Hg2+具有优异的识别能力,其识别机理为络合比1 : 1的可逆过程。

关键词:罗丹明B;2’-羟基苯乙酮;合成;Hg2+

中图分类号:06573.3     文献标识码:A    文章编号:0258-3283201*

 

Synthesis of Rhodamine-based Fluorescent Probe for Recognition of Hg2+ XIAO qian[1](College of Chemistry and Environmental Engineering,Hanshan Normal University,Chaozhou 521041, China), Huaxue Shiji, 2017, 39(10)

Abstract: A rhodamine-based mercuric ion fluorescent probe L was synthesized expediently by the condensation reaction of several inexpensive compounds such as rhodamine B, hydrazine hydrate and 2'-hydroxyacetophenone, and its structure was confirmed by 1HNMR、13CNMR and HRMS. Probe L has markedly recognition properties for mercuric ion in EtOH-H2O (V(EtOH)︰V(H2O)=4︰1, at pH 7.0, 20 mmol/L HEPES buffer) solution. The stoichiometry of L-Hg2+ complex was estimated to be 1∶1 and their recognition process was revisable.

Key words: rhodamine B; 2'-hydroxyacetophenone; synthesis; Hg2+

 

 

稳定同位素标记苏丹红-D5合成研究

卢浩,孙雯,徐仲杰*

(上海化工研究院 技术开发中心,上海 普陀  200062

 

摘要以廉价易得的苯-D6为起始原料,经硝化、还原、重氮化、偶合生成苏丹红I-D5。以消耗的苯-D6计算,苏丹红I-D5总收率可达82.2%。采用1HNMR和ESI-MS等确定产品结构信息,产品的同位素丰度为99.1 atom %D,纯度为99.5%。该化合物可作为应用于食品安全检测领域非法添加物质苏丹红I的检测的稳定同位素内标试剂。

关键词合成;稳定同位素;苏丹红Ⅰ-D5;食品安全

中图分类号:TQ431.6                文献标识码:A             文章编号:005918

 

Synthesis of Sudan-D5 Labeled with Stable Isotope LU Hao, SUN Wen, XU Zhong-jie* (Technology Development CenterShanghai Research Institute of Chemical IndustryShanghai 200062China)

Abstract:This work presents an efficient and convenient synthesis method of sudanⅠ-D5 with benzene-D6 as the common substrate, which is mainly obtained via nitration, reduction, diazotization and a coupling reaction. The yields of sudan-D5 was 82.2% based on benzene-D6 consumed. The product’s structures were confirmed by HNMR and ESI-MS. The chemical purity of this product is 99.5% and deuterium isotopic enrichment of this product is 99.1 atom% D. The compound could be used in the field of food safety testing as stable isotope internal standard reagent.

Key words: synthesis; stable isotope; SudanⅠ-D5; food safety

 


一种高效合成2--4-甲基磺酸-苯甲醛的方法

胡燕,刘希海,孙兵,张方林*

(武汉理工大学 化学化工与生命科学学院,湖北 武汉  430070

 

摘要:报道了一种高效合成2-氯-4-甲基磺酸-苯甲醛的方法。通过对溶剂、酸、临时导向基团和氯源的精确调控,可得到产量高达81%的邻位单氯取代产品。该优化体系可放大到克级,具有高活性和高选择性的特点。

关键词:4-甲基磺酸-苯甲醛;钯;临时导向基团;放大

中图分类号:TQ46       文献标识码:A        文章编号:0258-32832017

 

Efficient Synthesis of 2-Chloro-4-methanesulfonyl-benzaldehyde HU Yan, LIU Xi-hai, SUN Bing, ZHANG Fang-lin* (School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, China), Huaxue Shiji, 2017, 39(10)

Abstract: An efficient and practical method for the synthesis of 2-chloro-4-methanesulfonyl-benzaldehyde has been reported. By fine control over the solvents, acid, transient directing groups and chlorine sources, a yield of orthomonochloro-substituted product up to 80% was achieved. This optimized system can be scaled up in gram, with high activity and selectivity.

Key words: 4-methanesulfonyl-benzaldehyde;Pd;transient directing group;scale-up

 

 

 

新型降糖候选化合物ZG02的合成方法改进及其手性分离

杨宗圮,李述敏,李云艳,李小双,张吉泉*,王颖*,汤磊

(贵州医科大学 药学院,贵州 贵阳  550004)

 

摘要:研究发现新型四氢咔唑衍生物ZG02有较强的体内外降糖与降脂活性,是一个有深入开发价值的候选化合物。前期报道制备方法存在总产率低、纯化困难等问题。本研究经方法改进后以4-氧代环己酮羧酸为原料经烯丙基保护、Fischer-吲哚环合、酰化及脱保护等4步反应得到目标产物,总收率为71.9%。同时,利用手性制备柱对ZG02进行了拆分,得到了光学纯异构体,以便进一步评价不同构型异构体的生物活性差异。

关键词:四氢咔唑;降糖活性;合成;手性分离

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

 

Improvement on Synthesis of Novel Hypoglycemic Candidate ZG02 and Chiral Separation YANG Zong-pi, LI Shu-min, LI Yun-yan, LI Xiao-shuang, ZHANG Ji-quan*, WANG Ying*, TANG Lei (College of Pharmacy, Guizhou Medical university, Guiyang 550004, China)

Abstract: The work revealed that novel tetrahydrocarbazole derivative ZG02 possessed potent hypoglycemic and hypolipemic activities both in vitro and in vivo and thus, a promising candidate for the treatment of type 2 diabetes. The previous method suffered from low total yield and hard for purification. In this work, taking 4-oxocyclohexanecarboxylic acid as starting material, the title compound was synthesized via allylation, Fischer indole synthesis, acylation and deprotection with a total yield of 71.9%. Besides, a chiral separation on ZG02 and optically pure isomers were obtained via preparative column, and therefore provide samples for further bio-evaluations.

Key words:tetrahydrocarbazole; hypoglycemic activitie; synthesis; chiral separation

 

 

3, 5-二氯-a-(三氟甲基)苯乙烯合成工艺的改进

王勇a, b,刘明*a, b

(荆楚理工学院 a. 化工与药学院 药物合成与优化湖北省重点实验室,b. 化工绿色技术研究院,湖北 荆门  448000)

 

摘要:以3, 5-二氯溴苯为起始原料,在镁和二异丁基氢化铝等条件下制成格氏试剂后,再与三氟乙酸乙酯发生取代反应制得3′, 5′-二氯-2, 2, 2-三氟苯乙酮。然后,3′, 5′-二氯-2, 2, 2-三氟苯乙酮与甲基三苯基碘化磷在叔丁醇钾作用下发生Witting反应,制得目标产物3, 5-二氯-a-(三氟甲基)苯乙烯。通过对3′, 5′-二氯-2, 2, 2-三氟苯乙酮和3, 5-二氯-a-(三氟甲基)苯乙烯进行IR、MS、UV、1HNMR和13CNMR等表征,确认了化合物的结构。该合成路线具有操作简单、反应条件温和、原料便宜易得、绿色环保、成本低等优势。

关键词:格氏试剂;3, 5-二氯-a-(三氟甲基)苯乙烯;Witting反应;结构表征

中图分类号:O621.3        文献标识码:A      文章编号:0258-32832017

 

Synthesis of 1,3-Dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene WANG Yonga,b, LIU Minga,b*(a. Hubei Key Laboratory of Drug Synthesis and Optimization, College of Chemical Engineering and Pharmacy, b. Institute of Green Chemical Technology, Jingchu University of Technology, Jingmen  448000, China)

Abstract:In this work, 1-(3,5-dichlorophenyl)-2,2,2-trifluoroethanone was synthesized by reaction of ethyl trifluoroacetate with the Grignard reagent, which was obtained by reaction of 3,5-dichlorobromobenzene, magnesium and diisobutyl aluminum hydride. 1-(3,5-dichlorophenyl)-2,2,2-Trifluoroethanone was then reacted with methyltriphenylphosphonium iodide in the presence of potassium t-butoxide to give the desired product 1,3-dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene. Above two compounds were confirmed by IR, MS, UV, 1HNMR and 13CNMR. The synthetic route has the advantages of simple operation, mild reaction condition, cheap and easy access to raw materials, green environmental protection and low cost.

Key wordsGrignard reagent; 1,3-dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene; Witting reaction; structure characterized

 

 

药物中间体5-苄氧基-2-羟基苯甲醛的合成

郑苏*,沈新安

(江苏省徐州医药高等职业学校 制药工程系,江苏 徐州  221116

 

摘要:以对苯二酚和氯苄为起始原料,选用无水碳酸钾作缚酸剂、碘化钾作催化剂、乙腈作溶剂,合成对苄氧基苯酚,然后在三乙胺为缚酸剂、无水氯化镁为催化剂的条件下与多聚甲醛反应制备目标产物,两步反应总收率43.97%,产物经过1HNMR和MS确认。

关键词:对苯二酚;5-苄氧基-2-羟基苯甲醛;合成

中图分类号: 0622.4            文献标识码:A             文章编号:0258-3283201*

 

Synthesis of Drug Intermediate 5-Benzyloxy-2-hydroxybenzaldehyde ZHENG Su*SHEN Xin-an (Department of PharmaceuticlEngineering, Jiangsu Xuzhou Vocational College of Pharmaceutics, Xuzhou 221116, China)

Abstract: Firstly, p-benzyloxy phenol was synthesized by using hydroquinone and benzyl chloride as starting materials under potassium carbonate as an acid binding agent, and potassium iodide as catalyst. Then, anhydrous magnesium chloride as a kind of catalyst, triethylamineas an acid binding agent, 5-(benzyloxy)-2-hydroxybenzaldehyde was synthesized. The total yield was about 43.97%. The intermediate and target compound was confirmedby 1HNMR and MS.

Key words: hydroquinone; 5-benzyloxy-2-hydroxybenzaldehyde; synthesize

 

 

金催化硫醚C(sp3)−H键与二羧酸碘苯直接乙酰氧基化反应研究

范芳婷,陈建飞,方雪颖,刘月,欧阳婷,郭圣荣*

(丽水学院 化学化工系,浙江 丽水  323000

 

摘要:在金的催化作用下,甲硫基C(sp3)-H键与高价碘试剂碘苯二乙酸能直接发生乙酰氧基化反应,据此合成了一系列α-芳硫基取得的羧酸酯类衍生物。该合成路线具有反应时间短、催化剂用量低、选择性地与硫原子邻位的C (sp3)−H键发生官能化反应等优点。

关键词:高价碘;乙酰氧基化反应;金催化;硫醚

中图分类号:O626.2 文献标识码:A      文章编号

 

Gold CatalyzedDirect Acetoxylation of UnactivatedSulfidesC(sp3)-H Bonds FAN Fang-ting, CHENJian-fei, FANG Xue-yin, LIU Yue, OUYANG Ting, GUO Sheng-rong* (Department of Chemistry, Lishui University, Lishui 323000)

Abstract: A gold-catalyzed direct oxidative acetoxylation of C(sp3)-H bond via iodine(III)-mediated sulfides to synthesize various α-thioaryl or α-thioalkyl ester derivatives was discussed. The attractive feature of this protocol includes short reaction time, low catalyst loading, and in situ activation of the sulfur atom.

Key words: hypervalent iodine; acetoxylation; gold;sulfides

 

 

二噁英半抗原中间体合成的研究

杨夕强*苏鹏辰王冠蕾曹克广

(承德石油高等专科学校 化学工程系,河北承德 067000

 

摘要:二噁英类化合物是一类重要的持久性有机污染物,它对环境及人体的危害日益引起人们的关注。酶联免疫分析(ELISA)技术是实现高效检测环境中二噁英残留的重要方法,而酶联免疫分析的关键基础是半抗原的合成。对二噁英半抗原合成中的核心步骤进行了详尽的探索,确定了此类反应的最佳反应条件:反应温度为常温,甲苯为溶剂,碱为0.015 mol氢化钠,催化剂15-冠-5-醚的加入量为n(15-冠-5-醚)︰n(4-氯-3-硝基苯甲醛)=0.02︰1。

关键词:二噁英;检测;半抗原;合成

中图分类号:O626  文献标识码:A     文章编号:0258-32832017

 

Synthesis of Dioxins Haptens Intermediate ProductYANG Xi-qiang*, SU Peng-chen,WANG Guan-lei, CAO Ke-guang(Department of Chemical Engineering,ChengdePetroleumCollege, Chengde067000, China), Huaxue Shiji, 2017, 39(11)

Abstract: Dioxins is a kind of important persistent organic pollutants, and it arouses people's concern increasingly because of its harm to environment and human body. Enzyme-linked immunoassay (ELISA) technology is an important method to detect residual dioxins in the environment, and its key step is the synthesis of haptens. In this work, the reaction conditions of this key step have been explored and determined. The optimum reaction conditions were: room temperature, solvent is toluene, amount of sodium hydride is 0.015 mol, n(15-crown-5  ether): n(4-chloro-3-nitrobenzaldehyde)=  0.02 :  1.

Key words: dioxins; detect; haptens; synthesis