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《化學試劑》2019年第6期中英文摘要

發布時間: 2019-06-14 13:44:07   試劑信息網

穩定同位素氘標記試劑的研究進展

徐仲杰,雷雯,羅勇*

(上?;ぱ芯吭河邢薰?/span> 國家同位素工程技術研究中心上海分中心,上海  200062 )

 

摘要: 穩定同位素氘標記試劑是科研工作中必不可少的試劑。氘代溶劑可有效避免普通溶劑氫原子干擾,被大量用于核磁共振儀溶劑。氘標記內標試劑具有優良的示蹤效果,廣泛地應用于食品領域的農殘檢測、獸殘檢測、非法添加劑、藥物殘留檢測等方面。此外,由于氘原子的良好的化學惰性,氘標記試劑還用于新藥研發領域。穩定同位素氘標記試劑的合成方法主要有化學合成法及物理交換法。從核磁檢測、食品安全、生命科學、藥物研發等方面闡述國內外近幾年穩定同位素氘標記試劑的研發新技術以及應用展望。

關鍵詞: 穩定同位素;氘標記;合成;檢測;應用

中圖分類號: O652     文獻標識碼:A    文章編號:0258-32832019

 

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

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

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

 

硒催化綠色合成反應進展

俞磊

(揚州大學 化學化工學院,江蘇 揚州  225002

 

摘要:由于硒催化劑具有價格低廉、對生態友好、可回收利用、催化過程清潔等優點,硒催化的綠色合成反應有著很好的工業應用前景。最近5年以來,硒催化的有機化學反應被廣泛報道,著重研究了硒催化的綠色合成反應,利用該催化技術,開發了一系列綠色氧化方法,為制備很多精細化工中間體,如反式-1,2-環己二醇、2-取代環丁酮、烯酯、β-紫羅蘭酮環氧化物、有機腈、醛酮等,提供了新的合成方法。此外,通過對比分析各反應之間的聯系,已逐步探索出有機硒催化反應中選擇性調控的一般規律,提出了相關的理論。對相關研究進行了回顧,并展望了這一領域的發展趨勢。

關鍵詞:硒;催化;有機合成;綠色化學 

中圖分類號:O6         文獻標識碼 A          文章編號0258-32832019--

 

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

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

Key words Selenium; catalysis; organic synthesis; green chemistry

 

乙二醇催化氧化反應研究進展

寧宇峰,張建棟*,李興,魏文瓏,常宏宏,高文超*

(太原理工大學 生物醫學工程學院,山西 太原  030024 )

 

摘要:乙二醇屬于最簡單的二元醇,其化學性質活潑,可發生酯化、醚化、氧化、縮合、脫水等反應。針對乙二醇在近年來行情低迷,產能過剩的狀況,重點論述了以乙二醇為主要原料可進行的的氧化反應轉化,包括化學氧化法、電化學氧化法和生物催化氧化法。詳細分析了酶催化和靜息細胞催化等生物法轉化乙二醇合成乙醇醛、乙醇酸、乙二醛等的相關研究報道,指出了生物催化氧化法相較于傳統化學氧化無可比擬的優點,并對以乙二醇為原料合成精細化學品進行了展望。

關鍵詞:乙二醇;催化氧化;生物氧化

中圖分類號: O622.3    文獻標識碼: A    文章編號: 0258-32832019

 

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

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

Key words: ethylene glycol; catalytic oxidation; biological oxidation

 

氮雜環卡賓-(II)-1-甲基咪唑配合物催化苯并噁唑與對甲苯磺酸芳酯的C-H鍵直接芳基化反應

鄭宛瑩,劉青鮮,邵黎雄*

(溫州大學 化學與材料工程學院,浙江 溫州  325035)

 

摘要2-芳基苯并噁唑是一類非常重要的有機化合物。以氮雜環卡賓-(II)-1-甲基咪唑[NHC-Pd(II)-Im]配合物為催化劑,通過催化苯并噁唑與對甲苯磺酸芳酯的C-H鍵直接芳基化,高效合成了2-芳基苯并噁唑類化合物。使用0.05倍物質的量的NHC-Pd(II)-Im配合物為催化劑,3.5倍物質的量的LiOtBu為堿,以甲苯為溶劑,不同取代基的苯并噁唑和對甲苯磺酸芳酯在130 oC下反應12 h,以71% 92%的收率得到相應的C-H鍵直接芳基化產物。

關鍵詞:氮雜環卡賓鈀配合物;苯并噁唑;對甲苯磺酸芳酯;C-H芳基化

中圖分類號:O621.3    文獻標識碼:A    文章編號:0258-32832019

 

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

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

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

 

微通道混合器的研制及在微乳液制備中的應用

朱寶偉*,劉海燕,陳紅,馮若凡

(營口理工學院 化學與材料工程系,遼寧 營口   115014

 

摘要:微通道混合技術具備混合均勻可控制、傳質傳熱效率高等特點。采用COMSOL Multiphysics有限元分析軟件,通過建立微通道簡化模型,設置理想化參數模擬微通道傳質特點,根據理論分析與模擬結果進行了微通道混合器設計和加工。實驗選擇聚甲基丙烯酸甲酯(PMMA)為基本材質,設計、加工了三維立體結構的切割重組型號的微通道混合器,并用于微乳液復配實驗。微乳液復配實驗結果顯示微通道加工工藝可行,可用于油相水相的混合。

關鍵詞:微通道;傳質;模擬;加工;微乳液配制

中圖分類號TQ423      文獻標識碼A      文章編號0258-32832019--

 

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

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

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

 

 

7-二乙氨基香豆素-3-烯丙端基化合物的合成及其熒光性質研究

卜明a,王海君*a,馬玉坤b,王靜a,李爽a,陳頌a,劉磊a,孫靖文a

(齊齊哈爾醫學院 a.藥學院,b.醫藥科學研究院,黑龍江 齊齊哈爾  161006

 

摘要:以4-二乙氨基水楊醛、丙二酸環亞異丙酯為原料,經Knoevenagel反應生成7-二乙氨基香豆素-3-羧酸,與氨基酸發生縮合反應后與3-溴丙烯反應,設計合成了37-二乙氨基香豆素-3-烯丙端基化合物。結構經1HNMR、13CNMR、MS等加以表征,并對其熒光性質進行測定。結果表明,3種烯丙端基化合物收率均超過70%,熒光發射峰波長分別為489、498、508 nm,其中化合物3c具有相對較較大的Stokes位移,對A549細胞進行染色,綠光激發時,細胞呈現出強烈的綠色熒光,成功實現細胞內熒光成像,具有良好的生物應用前景。

關鍵詞7-二乙氨基香豆素-3-羧酸;3-溴丙烯;熒光;細胞成像

中圖分類號:O626.2     文獻標識碼:A      文章編號:0258-32832019

 

Synthesis and Fluorescence Properties of 7-Diethylamino Coumarin-3-allyl End Group Compounds BU Ming1,WANG Hai-jun*1,MA Yu-kun2,WANG Jing1,LI Shuang1,CHEN Song1,LIU-Lei1,SUN Jing-wen1 (1.College of Pharmacy, 2.Research Institute of Medicine & Pharmacy, Qiqihar Medical University, Qiqihar 161006, China), Huaxue Shiji, 2019,

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

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

 

 

納米碳酸鈣吸油值的研究

常迎星,王丹丹,鞏艷萍,牛振寧*,郭俊凌

(山西蘭花華明納米材料股份有限公司,山西 晉城,048002)

 

摘要: 納米碳酸鈣作為一種無機填料,其吸油值大小決定了納米碳酸鈣的表面化學性質、下游加工應用性能,吸油值越小,顆粒的分散性越好,加工性能越好。采用正交試驗法優選納米碳酸鈣的制備工藝,通過正交設計選取不同氫氧化鈣濃度、晶型導向劑添加量、改性劑添加量及改性時間,經過碳化合成法合成納米碳酸鈣,對其吸油值進行考察,并對實驗結果進行了極差分析。研究結果表明,影響納米碳酸鈣吸油值的主要因素是改性時間,其次是氫氧化鈣濃度。通過正交試驗得出最優的實驗條件為反應起始溫度為45 ℃時,氫氧化鈣濃度8.5%,晶型導向劑添加量0.9%,改性劑添加量3.5%,改性時間2 h,此時所得納米碳酸鈣吸油值為26.37。在最優條件下,所合成的納米碳酸鈣顆粒粒徑為50 100 nm,晶型為立方體形,邊界清晰,硅酮膠應用實驗擠出性27.36 g/min,流變性黏度0.62 mPa/s,觸變環面積2 334 Pa/s,屈服值133.56 Pa。

關鍵詞:正交實驗;納米碳酸鈣;氫氧化鈣濃度; 晶型導向劑; 改性; 吸油值

中圖分類號TQ115    文獻標識碼A     文章編號0258-32832019--

 

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

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

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

 

 

P21活化激酶-4及其抑制劑研究進展

李瑞娟1,程卯生2,王健*2

1.內蒙古醫科大學 藥學院,內蒙古 呼和浩特  010110;2. 沈陽藥科大學 基于靶點的藥物設計與研究教育部重點實驗室,遼寧 沈陽  110016

 

摘要: P21活化激酶4P21-activated kinase 4,PAK4)為小G蛋白Rho家族的關鍵下游效應器,通過多種機制影響腫瘤細胞的侵襲轉移、增殖、存活及凋亡,對腫瘤的發生發展起著重要作用。PAK4在多種腫瘤細胞中過度表達,并成為極具研究前景的藥物靶點。近年來,已經陸續發現了多種類型的PAK4激酶抑制劑,主要對PAK4激酶的結構特征、在腫瘤的發生發展中PAK4的作用機制以及PAK4激酶抑制劑的研究進展等做總結和闡述。

關鍵詞: P21活化激酶4;蛋白結構;作用機制;抑制劑;抗腫瘤藥物

中圖分類號R914       文獻標識碼A         文章編號:0258-32832019

 

Progress in PAK4 Kinase and Inhibitors LI Rui-juan1,CHENG Mao-sheng2,WANG Jian*2 1. College of Pharmacy, Inner Mongolia Medical University, Huhhot 010110, China; 2. Key Laboratory of Structure Based Drug Design & Discovery, Ministry of Education, Shenyang Pharmaceutical University, Shenyang 110016, China, Huaxue Shiji, 2019, 41(6)

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

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

 

Diels-Alder反應合成氧化吲哚螺環化合物研究進展

劉湘1,曹國銳1,2,李高寧*1

1.青島科技大學 化工學院,山東 青島  266042;2.濟寧市化工研究院,山東 濟寧  272000

 

摘要:氧化吲哚螺環化合物是多種天然產物的核心骨架,具有抗瘧、抗癌、避孕、抗高血壓等多種生物活性和藥物活性,因此受到有機化學家們的廣泛關注。目前報道的氧化吲哚螺環化合物的方法主要有1,3-偶極環加成反應、多組分串聯反應以及Diels-Alder反應等,其中Diels-Alder反應憑借其條件溫和、選擇性好等諸多優點,成為構建螺環化合物的高效方法。在手性催化和非手性催化兩方面闡述了通過Diels-Alder反應合成氧化吲哚螺環化合物的研究方法,根據催化劑的不同對其進行了分類和總結,最后對氧化吲哚螺環化合物合成的發展趨勢作出了展望。

關鍵詞:Diels-Alder反應;氧化吲哚螺環化合物;不對稱催化

中圖分類號:O621.3     文獻標識碼:A     文章編號:0258-32832018--

 

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

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

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

 

NMR技術測定口服液中葡萄糖酸含量

冷霄云1, 2,史淑丹1,李怡然2,朱明慧2,山廣志*2,劉曉娟*1

1.錦州醫科大學 藥學院,遼寧 錦州 121000;

2.中國醫學科學院北京協和醫學院醫藥生物技術研究所,北京 100050

 

摘要建立核磁共振氫譜定量(1H qNMR)分析方法,對葡萄糖酸鈣鋅口服溶液中葡萄糖酸進行含量測定。采用核磁共振譜儀,脈沖序列為zgpr,氘代水為溶劑,恒溫26.9 ℃;弛豫時間為20 s;采集時間為2 s;中心頻率為4.701 ppm;采集次數為32次。選擇δ 4.0  4.1處質子峰為葡萄糖酸定量峰,順丁烯二酸δ 6.3處為內標峰,m(葡萄糖酸):m(內標順丁烯二酸)在1.73 8.69范圍內線性關系良好,相關系數R2 0.9995;精密度、穩定性、重復性試驗的相對標準偏差(RSD)分別是1.87%、1.41%、1.83%;平均加樣回收率為99.62%,RSD 0.95%n 9)。建立的方法準確、簡便、高效,不需要使用對照品,可用于葡萄糖酸鈣鋅口服溶液制劑中葡萄糖酸的絕對定量。

關鍵詞:核磁共振氫譜定量;葡萄糖酸鈣鋅口服溶液;葡萄糖酸;順丁烯二酸

中圖分類號0482.532    文獻標識碼A        文章編號0258-32832019--

 

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

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

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

 

 

同位素稀釋質譜法測定土壤中氨基酸的含量

張鵬帥,侯捷,雷雯,杜曉寧*,侯靜華

(上?;ぱ芯吭?,上海  200062)

 

摘要:建立了同位素稀釋質譜法測定土壤中纈氨酸、亮氨酸、異亮氨酸、苯丙氨酸共4種氨基酸含量的檢測方法。通過在樣品中加入同位素內標試劑——穩定同位素15N標記的氨基酸,經酸解、固相萃取等前處理手段對目標氨基酸進行提取、富集以及衍生化后,利用GC-MS/MS多反應監測(MRM)模式進行定量分析。結果表明,在線性范圍內,4種氨基酸的線性相關系數(R2)均大于0.999,回收率為92.2%108%,方法檢出限(LOD)為1.42.9 μg/kg,定量限(LOQ)為5.28.8 μg/kg。方法高效、重現性好,可用于土壤中氨基酸的定量檢測。

關鍵詞:土壤中氨基酸;同位素稀釋;定量檢測;GC-MS/MS

中圖分類號:O657. 63    文獻標識碼:A     文章編號:0258-32832019

 

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

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

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

 

 

不同的萃取方式分析葫蘆巴浸膏揮發性成分

董振山1,黃世杰2,黃善松2,李慶祥1,李小蘭2,李志華2,胡志忠2,張峻松*1

(1.鄭州輕工業學院 食品與生物工程學院,河南 鄭州  450002;2.廣西中煙有限責任公司 技術中心, 廣西 南寧  530001)

 

摘要:為了明確葫蘆巴浸膏中揮發性成分組成、含量及不同萃取方式對葫蘆巴浸膏揮發性成分萃取效果的影響。分別采用固相微萃?。?/span>SPME)、溶劑萃?。?/span>LLE)和同時蒸餾萃?。?/span>SDE)對葫蘆巴浸膏中揮發性成分進行提取,利用GC-MS技術對揮發性成分進行分析鑒定。3種萃取方法共鑒定出160種揮發性成分,其中固相微萃?。?/span>SPME37種、溶劑萃?。?/span>LLE66種、同時蒸餾萃?。?/span>SDE113種,3種方式共有的16種,具有葫蘆巴浸膏特征香味成分的葫蘆巴內酯3種方式均能萃取出來,比較3種萃取方法可知:其中同時蒸餾萃?。?/span>SDE)和溶劑萃?。?/span>LLE)對葫蘆巴浸膏中香味物質提取的更為全面,兩種萃取方式共鑒定出151種。

關鍵字:葫蘆巴浸膏;溶劑萃??;固相微萃??;同時蒸餾萃??;GC-MS

中圖分類號:O657.7+1    文獻標識碼:A    文章編號:0258-32832019--

 

Analysis of Volatile Components of Fenugreek Extract via Different Extraction Methods for DONG Zhen-shan1, HUANG Shi-jie2, HUANG Shan-song2, LI Qing-xiang1, LI Xiao-lan2, LI Zhi-hua2, HU Zhi-zhong2, ZHANG Jun-song*1 (1. College of Food and Bioengineering, Zhengzhou University of Light Industry,Zhengzhou 450002, China;2. Technology Center, Guangxi China Tobacco Co., Ltd.,Nanning 530001, China), Huaxue Shiji, 2019, 41(5),

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

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

 

 水質污染監測用7種陰離子溶液標準物質的研制

張惠,張鵬輝,楊娜,高琴,方正*

(中國測試技術研究院,四川 成都  610021

 

摘要:使用電感耦合等離子體質譜儀、離子色譜儀等對研制的7種陰離子溶液標準物質原料的雜質進行定性和定量測定。通過雜質扣除法對原料純度定值,并定量測定原料中7種離子間相互包含情況。采用重量-容量法對溶液標準物質準確定值。7種陰離子溶液可用于測定7種陰離子的分析方法確認與評價、成分定量分析等。為復雜微量樣品中7種陰離子的測試參數提供參考標準??梢怨澕s監測資源、提高效率。對監測環境水、飲用水和食品中重要陰離子和盡量保證樣品檢測的及時性具有重要意義。

關鍵詞:陰離子;標準物質;雜質扣除法;復雜樣品

中圖分類號:O625. 11      文獻標識碼:A      文章編號:0258-32832019--

 

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

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

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

 

 

人參皂苷Rg3體外經皮滲透特性研究

史淑丹1,鄭巖1,王碩2,富力2,孫玉琦*1

(1. 錦州醫科大學 藥學院,遼寧 錦州  121001;

2. 大連富生天然藥物開發有限公司,遼寧 大連  116600)

 

摘要:研究人參皂苷Rg3體外經皮滲透特性以及不同促滲劑的影響。測定人參皂苷Rg3與經皮滲透相關的物理參數。通過擴散池試驗,采用HPLC法測定人參皂苷Rg3的累積透過量(Q),擬合Q-t曲線,考察體外經皮滲透性能;測定β-環糊精、吐溫-80、油酸、氮酮、薄荷油的增滲倍數(ER),考察不同促滲劑對人參皂苷Rg3經皮滲透性質的影響。人參皂苷Rg3的表觀溶解度為56.70 μg/mL,油水分配系數(logP)為2.63,熔點為312.2 ℃。人參皂苷Rg3經皮滲透為恒速過程,12 h累積透過量為14.45 μg/cm2;不同促滲劑對人參皂苷Rg3的促滲作用存在差異,薄荷油增滲倍數為2.38。人參皂苷Rg3體外釋放符合零級過程,薄荷油對其促滲作用效果顯著,可作為一種具有發展潛力的新型外用鎮痛化合物。

關鍵詞:人參皂苷Rg3;經皮滲透;促滲劑;累積透過量;增滲倍數

中圖分類號:R944.9    文獻標識碼:A       文章編號:0258-32832019

 

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

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

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

 

 

五爪金龍吸附陽離子染料的性能研究

楊新周a,b,楊子仙a,田先嬌b,c,馬艷粉b,c

(德宏師范高等??茖W校 a. 理工系,b.民族醫藥研究所,c. 生命科學系,云南 德宏  678400)

 

摘要:以五爪金龍為原料,經粉碎制成不同粒徑的粉末吸附劑,探究了五爪金龍吸附亞甲基藍、羅丹明B、堿性品紅的性能。研究發現,五爪金龍吸附亞甲基藍、羅丹明B、堿性品紅最佳粒徑為0.3 mm、最佳投加量分別為1.6、2.6、0.8 g,pH均為5、溫度為30 ℃、震蕩時間均為40 min。利用準一級、準二級動力學方程模擬五爪金龍吸附亞甲基藍、羅丹明B和堿性品紅的動力學過程,結果表明五爪金龍吸附亞甲基藍、羅丹明B和堿性品紅的過程適合于準二級動力學模型。研究熱力學參數發現,五爪金龍吸附亞甲基藍、堿性品紅的過程是一個自發的趨于無序的放熱過程,吸附羅丹明B的過程是一個自發的趨于有序的放熱過程。

關鍵詞:五爪金龍;亞甲基藍;堿性品紅;羅丹明B;吸附

中圖分類號:X703    文獻標識碼:A    文章編號:0258-32832019

 

Adsorptive Performance of Ipomoea Cairica on CatioIlic Dye in Aqueous Solution

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

Abstract:The powder of Ipomoea cairica at different particle sizes was prepared as adsorbent by crush. The adsorption properties of Ipomoea cairica powder for methylene blue, rhodamine B and basic fuchsine were investigated at various conditions. It showed that the optimal adsorption conditions were as follow: the dosage of Ipomoea cairica powder were 1.6、2.6、0.8 g, pH value were 5, particle size were 0.3 mm, adsorption time at 40 min and temperature at 30 . The pseudo-first-order, pseudo-second-order were used to simulate the kinetic process of it. The results showed that the pseudo-second kinetic equation is more suitable for describing the process of it. The thermodynamic parameters were calculated and results were as follow: in the process of Ipomoea cairica powder adsorption of methylene blue and basic fuchsine, which indicate that it is a spontaneous, disorderly and endothermic process. In the process of Ipomoea cairica powder adsorption of rhodamine B, which indicate that it is a spontaneous, orderly and endothermic process.

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

 

 

雜多酸離子液體催化下的過氧乙酸綠色合成工藝研究

胡珂1,康麗峰2,余定華*2

(1.  南京市第一中學,江蘇 南京  210001;2. 南京工業大學 藥學院,江蘇 南京  210009

 

摘要: 以溴化1-丁基-3-甲基咪唑([Bmim]Br)和磷鎢酸(H3PW12O40)為原料制備了雜多酸型離子液體催化劑1-丁基-3-甲基咪唑磷鎢酸鹽([ Bmim]3PW12O40),經傅里葉變換紅外光譜確證其結構,考察了催化劑對雙氧水氧化冰醋酸合成過氧乙酸反應的催化活性及其催化工藝條件。實驗結果表明,該雜多酸離子液體是一種新型、高效且環境友好的固相催化劑,在:V(雙氧水)∶V(冰醋酸)=1.751、溫度 60 ℃、催化劑用量為原料總質量的0.5%、時間4 h的優化反應條件下,過氧乙酸的濃度可達到20.3%。而且,催化劑循環使用8次后,依然保持了優異的穩定性。制備的過氧乙酸產品因不含硫酸催化劑,解決了現有濃硫酸催化方法存在的環境不友好、儲存和運輸存在安全隱患、產品應用領域受限等問題。

關鍵詞:離子液體;磷鎢酸;雜多酸;過氧乙酸;綠色合成

中圖分類號:TQ111    文獻標識碼:A       文章編號:0258-32832019

 

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

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

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

 

 

7-氮雜吲哚及其衍生物5--7-氮雜吲哚的合成

鄭從燊1,陳夏琴1,余輝1,黃捷*1,楊帆2,湯杰2

(1. 福建省微生物研究所,福建 福州  350007; 2. 華東師范大學 化學與分子工程學院,上海  200241)

                                                                                                                                                 

摘要7-氮雜吲哚是一種重要的雜環化合物,是合成維羅非尼、ABT-199等抗腫瘤藥物的重要中間體,具有較高的生物醫藥價值。優化了合成7-氮雜吲哚的方法,以廉價易得的2-氨基-3-甲基吡啶為起始原料,經過兩步反應,以48%的總收率得到7-氮雜吲哚。并在此合成方法的基礎上進一步合成了5--7-氮雜吲哚,經過三步反應,總收率達到43%。該合成方法具有原料易得、操作簡便、路線簡短、收率較高等優點。產物的結構經過核磁共振和高分辨質譜得到確認。

關鍵詞:7-氮雜吲哚;5--7-氮雜吲哚;雜環;合成

中圖分類號: O626.32               文獻標識碼:A             文章編號:0258-32832019

 

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

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

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

 

 

C22-脂環族三羧酸()的合成工藝改進

廖德仲1,占達東2,孫宏元2,趙玉玲2,何節玉*2

(1. 湖南理工學院 化學化工學院,湖南 岳陽  414000;2. 海南熱帶海洋學院 海洋科技學院,海南 三亞  572022)

 

摘要:介紹了一種生物基多官能團有機酸―C22-脂環族三羧酸()的改進合成工藝,并與其相關的文獻報道進行了比較。在單質碘的催化作用下,從海蓬籽油制備的共軛亞油酸與順丁烯二酸酐進行Diels-Alder反應合成了上述產物;通過L9(34)正交試驗優化了合成工藝條件;選用正庚烷為溶劑分離產物,并經FTIR、MSNMR證實。正交試驗得到的優化工藝條件為:順丁烯二酸酐與共軛亞油酸的物質的量比為1.2、催化劑用量0.2 wt %、反應溫度60 °C、反應時間2.0 h,此條件下產率高達96.5%。本改進合成工藝具有低溫、常壓、高效、產物分離相對簡單等優點。

關鍵詞:海蓬籽油;共軛亞油酸;C22-脂環族三羧酸();Diels-Alder反應;改進合成

中圖分類號:O624.5     文獻標識碼:A      文章編號:0258-32832019--

 

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

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

 

N-氨基磺?;纂哳惢衔锏暮铣裳芯?/span>

伍悅瑄,阿不都熱合曼·烏斯曼*

(新疆師范大學 化學化工學院,新疆 烏魯木齊 830054

 

摘要:以二氯甲烷為溶劑,甲酰胺在三氯氧磷的活化作用下生成活性中間體,再與N-氨基磺酰胺發生縮合反應生成一系列的目標化合物,并通過紅外光譜(FT-IR),核磁共振(NMR)和高分辨質譜(HR-MS)等分析方法進行結構表征。討論了鹵化試劑、溫度、溶劑以及反應物投料比對產率的影響。結果表明,最佳反應條件為:三氯氧磷作為鹵化試劑,二氯甲烷為溶劑,nN-氨基磺酰胺):n(甲酰胺) 11.5,溫度為40 ℃,目標化合物的最高產率可達到95%。

關鍵詞N-氨基磺酰脒,N-氨基磺酰胺,三氯氧磷,甲酰胺

中圖分類號O626     文獻標識碼A     文章編號0258-32832019--

 

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

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

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

 

木耳狀g-C3N4的合成

王俊林a,張亞娜a,李夢佳a,李小妹a,常玥*a,b,查飛a

(西北師范大學 a.化學化工學院, b.生態環境相關高分子材料教育部重點實驗室, 甘肅 蘭州  730070)

 

摘要:以三聚氰胺、三聚氯氰為原料,550 ℃熱聚合法制備了g-C3N4(FCN)。13C NMR、XRD證明該g-C3N4的結構單元是3-s-三嗪環。電鏡照片顯示FCN形貌為木耳狀,邊緣較厚。原料三聚氯氰、三聚氰胺分別是4 g、2 g時,N2吸附-脫附測定FCN1的比表面積為156.25 m2/g,孔徑60 nm。UV-vis漫反射測試FCN1的吸收邊緣為482 nm,對應禁帶寬度2.57 eV,PL光譜顯示FCN1光致發光強度最弱。可見光照射下,30 mg FCN1加入30 mL30 mg/L)的羅丹明BRhB)溶液中,50 minRhB的光降解率是99.6%,光催化劑循環實驗表明該木耳狀g-C3N4具有良好的穩定性。

關鍵詞:g-C3N4;木耳狀;高比表面積;光催化;RhB

中圖分類號:O643.36   文獻標識碼:A    文章編號:0258-3283(2019)--

 

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

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

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

 

 

硝基烯烴與丙二酸酯的Michael加成反應研究

林敬a, b,徐立杰b,范欣然b,劉兆芳b,潘婷b,戴兢陶*b

(鹽城師范學院 a.分析測試中心,b.化學與環境工程學院,江蘇 鹽城  224007)

 

摘要:β-CF3-β-(3-吲哚)硝基烯烴衍生物和丙二酸酯為反應起始原料,在碳酸銫堿性條件下,用甲苯作為反應溶劑,于35 ℃下攪拌反應,實現了β-CF3-β-(3-吲哚)硝基烯烴衍生物與丙二酸酯的Michael加成反應。通過對堿、反應溶劑、堿的用量、底物濃度和反應溫度等因素的考察,確定了反應的最優條件。然后,在最優條件下,實現了不同結構的β-CF3-β-(3-吲哚)硝基烯烴與丙二酸酯的Michael加成反應,以最高95%的收率獲得了既含三氟甲基又含吲哚片段的γ-硝基丁酸酯,其結構均經過1HNMR、13CNMR、ESI-HRMSIR確證。

關鍵詞:β-CF3-β-(3-吲哚)硝基烯烴;丙二酸酯;Michael加成反應;γ-硝基丁酸酯

中圖分類號:O626.1        文獻標識碼:A           文章編號:0258-32832019

 

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

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

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

 


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