青藤碱衍生物合成研究进展

青藤碱是从植物青风藤中分离得到的异喹啉类生物碱,具有抗炎、免疫、镇痛、降压、抗心律失常等多种生理活性,用于治疗类风湿性关节炎及心律失常等疾病。但其用药剂量较大,且存在过敏等副作用,对其进行结构修饰,寻找高效低毒的青藤碱衍生物具有重要意义。本文从对青藤碱A、B、C、D四个环上活性基团的结构修饰出发概述了青藤碱衍生物的合成研究方法。     

一类偶氮苯酚类化合物的合成及表征

以取代苯胺为原料,经重氮化后与取代苯酚偶联合成了5个偶氮苯酚类化合物,产物经FTIR、1 HNMR表征。结果表明,产物结构与预期一致。     

偶氮苯二甲酰氯的合成和表征

以偶氮苯二羧酸和五氯化磷为原料,二氯乙烷为溶剂,三乙胺为酸吸收剂,合成了4种偶氮苯二甲酰氯,产率为75.3～93.6%。用红外光谱、核磁共振谱及元素分析进行了表征。     

青藤碱体内外微透析回收率的研究

目的:研究微透析探针对青藤碱体外回收率的影响因素和体内回收率的稳定性,为利用微透析技术进一步研究青藤碱关节腔局部的药动学提供依据.方法:采用液质联用技术(LC-MS)测定微透析样品浓度,运用增量法考察不同药物浓度、不同灌流速度对青藤碱体外回收率的影响,运用减量法考察青藤碱体内回收率在24h内的稳定性.结果:所建立的LC...     

青藤碱衍生物的合成及其体外抗炎活性研究

通过计算机辅助系统,模拟青藤碱与蛋白P50活性腔周边对接情况,以盐酸青藤碱为起始化合物,先发生Wohl-Ziegler反应,再通过钯催化的Suzuki偶联反应对其进行修饰,得到12个新型青藤碱衍生物,其结构经~1HNMR、~(19)FNMR、LC-MS等表征;采用报告基因法研究青藤碱衍生物对NF-κB转录活性的影响。12个青藤碱衍生物对NF-κB的转录活性均有一定的抑制作用,且抗炎活性优于青藤碱对照品。对青藤碱A环1位进行修饰可以提高抗炎活性,证明该作用靶点可进行深入探讨研究。     

含偶氮苯结构树枝状化合物的合成与表征

以间二苯甲酸为原料,经多步反应合成5-[4-（羟乙氧基苯基）偶氮]-1,3-苯二甲酸;进一步与均苯三甲酰氯反应得到新型含偶氮苯结构树枝状化合物,通过FT—IR、UV—vis和。HNMR对中间体及树枝状产物进行了结构表征。TGA分析显示,5％失重温度为225℃,DSC测得树枝状化合物的玻璃化转变温度（嗜）为95．7℃。     

一种末端单炔偶氮苯化合物的合成与表征

采用偶氮偶连、Williamson醚合成法,合成了一种末端单炔类偶氮化合物。通过红外光谱（FT-IR）、核磁共振（1H-NMR）对其结构和性能进行了表征。     

偶氮苯水杨醛缩氨基芴席夫碱的合成与表征

以苯胺和取代苯胺为原料,经重氮化、亲电取代以及缩合反应,设计合成了4种新型结构的偶氮苯水杨醛缩氨基芴席夫碱。经乙醇重结晶,以高达87.2%的产率得到目标产物,并利用~1HNMR、~(13)CNMR、红外光谱和元素分析对目标化合物的结构进行表征。     

偶氮卟啉的合成、表征与光电导性能

以对硝基苯甲醛和吡咯为原料合成了对硝基苯基卟啉,再经硝基还原、重氮化和偶合反应合成了两种多偶氮连接的卟啉化合物,并用核磁、质谱、红外光谱及紫外-可见光谱对化合物进行了结构表征.分别以这些卟啉化合物为电荷产生材料制备了功能分离型双层光电导体,并对其光电导性能进行了研究.结果表明,偶氮卟啉的光敏性明显优于四苯基卟啉,其光敏性分别为1.8和28.8 lx•s.     

一种末端双炔类偶氮苯化合物的合成与表征

采用偶氮偶联、金属钯催化偶联法和Williamson醚合成法,合成了一种末端双炔类偶氮化合物,其结构经IR、1H NMR、DSC分析表征.     

New Polymer Syntheses Part 53. Novel Polyamides of Diarylidenecycloalkanone Containing Azo Groups in the Polymer Backbone: Synthesis and Characterization

A new interesting class of polyamides of diarylidenecycloalkanone containing azo groups in the polymer backbone 6 _a-d was synthesized by a solution polycondensation reaction of bis 2-aminoarylidene monomers 3 _a,b with 4,4′-azodibenzoyl dichlorides and 3,3′-azodibenzoyl dichlorides in NMP as a solvent, using anhydrous LiCl as a catalyst at room temperature. The model compounds 4, 5 were synthesized by the interaction of one mole of bis 2-aminoarylidene monomers 3 _a,b with two moles of benzoyl chloride using anhydrous LiCl as a catalyst in NMP at room temperature. The resulting polymers were characterized by elemental and spectral analyses, besides solubility and viscometry measurements. The thermal properties of those polymers were evaluated by TGA, DTG and DTA measurements and correlated to their structural units. X–ray analysis of the polymers showed that polyamides based on para-azo linkage have a higher degree of crystallinity than those based on meta-azo linkage in the region 2θ = 5?60°. In addition, the morphological properties of selected examples were tested by SEM.      

双氰乙基偶氮化合物的合成及表征

用无水AlCl3催化问甲苯胺与丙烯腈的加成反应,合成了偶合组分N,N-二氰乙基间甲苯胺,并分别与重氮组分对硝基苯胺、对硝基邻氯苯胺、2,4-二硝基-6-氯苯胺和2,4-二硝基-6-溴苯胺进行偶合反应,合成了4种双氰乙基偶氮化合物.结果表明,生成的偶氮化合物产率分别为72%、78%、91%和81%,含量均超过96%;而且...     

稀土金属络合染料的合成研究

本论文选择1-对氯苯基-3-乙基-5-吡唑酮作为偶合组分,与3-氨基-4-羟基苯磺酰胺重氮组分反应合成偶氮染料母体,合成的母体染料与稀土络合剂反应生成稀土金属络合染料。利用红外光谱、紫外可见吸收光谱对合成的金属络合染料进行了结构鉴定与分析。本论文对络合反应条件进行了详细的研究,合成1∶2偶氮金属络合染料反应体系的pH值在8.0～8.5之间,反应温度75℃,偶氮金属络合染料的收率达90%以上。     

Synthesis and characterization of high molecular weight side chain liquid crystalline/photoactive polymers

Various liquid crystalline and photoactive azobenzene monomers were synthesized and attached to copoly(methyl methacrylate‐glycidyl methacrylate) [copoly (MMA‐GMA)] to get high molecular weight side chain liquid crystalline (LC)/photoactive copolymers. Further, spacers are generated in situ and reactive groups are obtained after the modification. All monomers and polymers were thoroughly characterized by FTIR, ¹H and ¹³C NMR, UV‐VIS spectrophotometry, gel permeation chromatography, thermogravimetric analysis, differential scanning calorimetry, and polarized optical microscopy. All side chain LC polymers showed higher thermal stability than that of copoly(MMA‐GMA). Three LC and one azo monomer exhibited characteristic nematic mesophase where as one LC monomer has shown nematic and sanded smectic‐A texture. The rate of trans‐cis isomerization of polymer was lower than that of the monomer and both monomers and polymers showed slow back isomerization. Present approach offers convenient way to synthesize high/desired molecular weight photoactive LC polymers. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

三种偶氮化合物的合成及三阶非线性光学性能

文章选取具有非线性光学活性的偶氮化合物作为研究对象,合成了一组含不同取代基和不同推-拉电子结构的偶氮化合物,并通过红外光谱、紫外-可见吸收光谱、元素分析、核磁共振氢谱等方法对所合成的偶氮化合物结构进行了表征;用单光束Z-扫描的方法对所合成的偶氮化合物的三阶非线性光学性能进行了测试,并结合理论计算分析研究了分子结构对偶氮化合物三阶非线性光学性能的影响。     

新型树枝状硅碳烷液晶大分子的合成与表征

以肌醇为核心 ,经烯丙基醚化、多步硅氢化加成反应和Grignard反应合成了树枝状大分子 3G -Cl,然后和偶氮苯介晶基元反应制备了新型树枝状硅碳烷液晶 ,用元素分析、核磁共振谱、激光飞行质谱对其进行了结构表征 ,偏光显微照片和差示扫描量热表明 ,其液晶相为向列型N相     

偶氮苯甲酸类衍生物的合成、表征及光学性能研究

设计合成了三种偶氮苯甲酸类化合物,产率均达84%以上.通过元素分析、1H NMR、MS及红外光谱对产物进行了表征,结果与预期产物吻合.通过紫外光谱和荧光光谱研究化合物的光学性能,发掘偶氮苯甲酸类化合物的光学特性与应用.     

丙环唑的合成及表征

以2,4-二氯苯乙酮、1,2-戊二醇、溴水、1,2,4-三氮唑等为主要原料,采用先环化后溴化再缩合的方法制备丙环唑成品,丙环唑粗品含量为94%~95%,采用酸碱中和去除杂质,生成的丙环唑硝酸盐,用液碱中和还原,得到纯的成品。其收率为72%丙环唑,比文献值提高了3%,采用此方法原料成本低,工艺条件简单,环境污染小,易于操作。     

Synthesis,characterization, and thermo‐optical properties of azobenzene polyurethane containing chiral units

An optically active levoazobenzene polyurethane (PU) was synthesized and was based on the chromophore 4‐(4′‐nitrophenylazo) phenylamine, the chiral reagent L (?)‐tartaric acid, and toluene diisocyanate. The chemical structure and thermal properties were characterized by ultraviolet–visible spectroscopy, Fourier transform infrared spectroscopy, ¹H‐NMR spectroscopy, and differential scanning calorimetry. The PU had high number‐ and weight‐average molecular weights up to 52 300, a large glass‐transition temperature of 235.7°C, and an optical rotation of ?18.06°, The optical parameters, including the refractive index (n) and thermo‐optic coefficient (dn/dT); the dielectric constant (?) and its variation with temperature; and the thermal volume expansion coefficient and its variation with temperature of PU were obtained. The dn/dT and ? values for the polymer were in the range ?4.1200 to 3.6257 × 10^?4 °C^?1 and 2.00 ± 0.11, respectively. The dn/dT values were one order of magnitude larger than those of inorganic glasses, such as zinc silicate glass (5.5 × 10^?6 °C^?1) and borosilicate glass (4.1 × 10^?6 °C^?1), and were larger than organic materials, such as polystyrene (?1.23 × 10^?4 °C^?1) and poly(methyl methacrylate) (?1.20 × 10^?4 °C^?1). The ? values were lower than that of alicyclic polyimide and semiaromatic polyimide. The obtained PU is expected to be useful for optical switching and optical waveguide areas. The conclusion has a little significance for the development of a new digital optical switch. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

几种8—氨基喹啉偶氮衍生物的合成及其与钴的显色反应研究

合成了４种多取代的８－氨基喹啉偶氮类新试剂。研究了它们与钴（Ⅱ）的显色反应。在表面活性剂的存在下,试剂与钴（Ⅱ）均有较高的反应灵敏度。对５－［（２－羧基－４－硝基苯基）偶氮］－８－氨基喹啉（ＮＣＰＡＱ）与钴（Ⅱ）的显色反应进行了较为系统的研究,配合物的吸收峰位于６６０ｎｍ,摩尔吸光系数为１．１５×１０５Ｌ·ｍｏｌ－１·ｃｍ－１,钴的量在０～１５μｇ／２５ｍＬ范围内符合比尔定律。