2-(5-芳氧基-4-苯基-1,2,4-三唑-3-硫基)乙酰芳胺的水相合成、 晶体结构及生物活性

在无催化剂存在下, 以水为溶剂通过5-芳氧基-4-苯基-1,2,4-三唑-3-硫酮与氯乙酰芳胺的硫烷基化反应, 合成了14个未见文献报道的2-(5-芳氧基-4-苯基-1,2,4-三唑-3-硫基)乙酰芳胺. 其结构经元素分析, IR和1H NMR进行了表征, 利用单晶X射线衍射法测定了化合物5n的单晶结构. 该化合物通过分子间氢键自组装成三维网状结构的超分子. 生物活性试验表明部分化合物对小麦的根有促进作用而对所有的茎都有抑制活性.     

α-氨基苯基膦酸酯衍生物的合成

以苯基二氯化膦为原料,合成了O-丁基苯基亚膦酸酯(1)。利用1中的P-H键与芳醛,芳胺的类M an-n ich反应,一锅煮合成了一系列具有多种潜在生物活性的新型α-氨基苯基膦酸酯(4)。1和4的结构经1H NMR,IR和MS确证。     

铜催化的多组分反应合成二芳基炔丙胺类衍生物

以醛、苯乙炔和二芳胺为原料, 三组分一锅法合成了一系列二芳基炔丙胺类化合物. 产物的结构通过1H NMR, 13C NMR和HRMS证实.     

一种星型有机低聚物的合成及光电性能

通过多步反应合成了一种新型的具有“双极(bipolar)”性质和发光性能的以N原子为中心的星型有机小分子低聚物——三(4-(5-(4-(5-(4-(二苯胺基)苯基)-1,3,4-噁二唑-2)苯基)-1,3,4-噁二唑-2)苯基)胺. 用¹H NMR, MS和元素分析进行了表征, 研究了化合物的热稳定性和固体粉末的光致发光性质, 并用循环伏安法测定了其电化学性能. 结果表明, 这种合成的同时具备空穴传导和电子输入双重功能基团的星型有机小分子光致发光性能优良(量子效率92%), 热稳定性好, 可以作为制作有机电致发光器件的候选材料.     

5-芳胺-6-氯-2, 3-二氰吡嗪的合成

本文以丙二腈为起始原料, 经过六步合成了中间体7, 化合物7和芳胺发生单取代得到目标产物5-芳胺-6-氯-2, 3-二氰吡嗪(8), 所合成的这10个目标产物文献上未见报道的, 通过了元素分析, IR, 1HNMR, MS证实其结构。粉末法测试表明它们都具有一定的二阶倍频效应。     

1-苯基-3-甲基-5-芳氧基-1H-吡唑-4-甲醛-O-[(2-氯吡啶-5-基)甲基]肟的合成与生物活性

利用1-苯基-3-甲基-5-芳氧基吡唑4-甲醛肟与2-氯-5-氯甲基吡啶发生缩合反应,合成了14个新型含吡啶环的吡唑肟醚衍生物.通过1H NMR,13C NMR和元素分析对所合成的化合物进行了结构表征.初步生物活性测试结果表明,在试验浓度下部分化合物具有一定的杀菌和植物生长调节活性.     

5-氨基-4-甲基噻唑-2-甲酰芳胺类化合物的合成及其生物活性

以拌种灵结构为先导,设计并合成了17个5-氨基-4-甲基噻唑-2-甲酰芳胺拌种灵类似物,其结构均经1H NMR,13C NMR,HRMS及IR确证.初步离体生物活性测试结果表明,大多目标化合物的杀菌活性高于对照物拌种灵.其中1个化合物对番茄早疫的杀菌活性是对照样拌种灵的2.6倍;5个化合物对黄瓜枯萎的杀菌活性是拌种灵的2倍以上.16个化合物对西瓜炭疽和水稻恶苗的杀菌活性均高于阳性对照,其中7个化合物对西瓜炭疽的杀菌活性高于阳性对照一倍以上.     

3-芳基-4-芳胺甲基异噁唑衍生物的合成及其生物活性初探

异噁唑衍生物由于其良好的生物活性一直受到有机合成化学家的关注,例如异噁唑衍生物具有杀虫、杀菌等生物活性.以3-芳基4-异噁唑甲酸乙酯为原料,经还原、溴化、取代反应合成了一系列3-芳基-4-芳胺甲基异噁唑衍生物,目标化合物结构经过~1H NMR、~(13)C NMR、HRMS鉴定.初步的生物活性测试结果显示,部分化合物对蚜虫和粘虫具有较好的抑制率.     

酰基硫脲衍生物的合成、结构表征及生物活性研究

在超声波辐射下, 以PEG-400为固-液相转移催化剂, 用芳胺与双酰基异硫氰酸酯反应, 合成出了15种新的结构不对称的双酰基硫脲类化合物(6和6')和9种新的分子中含酰胺基团的单酰基硫脲类化合物(7和7'). 利用元素分析, IR, ¹H NMR, ¹³C NMR, APT, 1D NOE及2D NMR技术确定了所合成化合物6和6'及7和7'的结构, 并对它们NMR谱中低场C, H进行了归属. 杀菌、杀虫和除草活性筛选测定实验结果表明, 所测试化合物对瓜炭疽病菌均具有抑制作用, 其中6e抑制率最高, 达到62.4%; 目标化合物7a对黄瓜白粉病菌有一定的抑制作用. 单胺氧化酶活性测定实验表明：大部分目标化合物对单胺氧化酶具有一定的抑制活性, 其中浓度在1×10^－3 mol•L^－1时目标化合物6'c和6'd的抑制活性较强, 明显高于其它化合物. 目标化合物没有抗惊厥活性.     

2,3-二芳基-1,3-苯并噁嗪的合成及杀菌活性

在三甲基氯硅烷(TMSCl)的催化作用下,取代苯甲醛与邻(芳胺甲基)苯酚经N杂缩醛化反应生成了一系列2,3-二芳基-1,3-苯并噁嗪类化合物。 目标化合物的结构用IR、¹H NMR、¹³C NMR和元素分析等技术手段进行了表征。 对所合成的化合物进行了初步杀菌活性测试,部分表现出良好的杀菌活性,化合物6e对菌核病菌的抑制活性为79.0%,化合物6a和6d均为74.8%,化合物6e对灰霉病菌的抑制活性为77.9%。     

Synthesis and properties of novel hole-transporting materials with triphenylamine units

Two novel organic hole-transporting materials have been synthesized by combination of triphenylamines(TPA) viaπ-conjugated bonds using Wittig reaction.The structures were characterized by NMR,FT-IR and HRMS.The optical,electrochemical and thermal properties of the materials were studied in detail.The results show that these two compounds have blue emission,proper HOMO levels and high thermal stability.Furthermore,a quantum chemical calculation on electron distribution of the two compounds was performed, which suggests the current synthesized materials would be promising candidates for hole-transporting materials.     

Synthesis and properties of new luminescent hole transporting materials of triarylamine with dehydroabietic acid methyl ester moieties

A series of triarylamines based on dehydroabietic acid methyl ester moieties (6a–h) were synthesized for possible application as hole transporting materials for organic electroluminescent devices. The target compounds were characterized by elemental analysis, FT-IR, NMR, and mass spectrometry. Their optical, electrochemical, and thermal properties were investigated using UV–vis, PL spectroscopy, cyclic voltammetry (CV), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC), respectively. CV measurements show that the compounds present suitable HOMO values (in a range of −4.63 to −5.11 eV) for hole injection, which is confirmed by theoretical calculations. All compounds were thermally stable. Organic light-emitting diode devices having 6f, 6g, and 6h as a hole transporting layer showed better performance of maximum brightness, turn-on voltage, and maximum luminous efficiency than a comparable device NPB. These compounds could be excellent candidates for applications in OLED devices.     

1,2-亚乙基桥联咔唑和芳基噁二唑的双极传输材料的合成及光电性能研究

设计合成了三种1,2-亚乙基桥联咔唑和2,5-二芳基-1,3,4-噁二唑衍生物的双极传输材料,并通过核磁氢谱、碳谱、元素分析表征了它们的分子结构,研究了它们的紫外-可见吸收、光致发光、电化学和热稳定等性能.研究结果表明,这类双极传输材料具有咔唑和芳基噁二唑双功能基的紫外可见吸收和光致发光综合特性.热分解温度超过了340℃.与共轭基团桥联咔唑和芳基噁二唑的双极传输材料相比,HOMO/LUMO能级相应地提高,热稳定性能增强.     

Liquid triarylamines: the scope and limitations of Piers-Rubinsztajn conditions for obtaining triarylamine-siloxane hybrid materials

New liquid triarylamine-siloxane hybrid materials are produced using the Piers-Rubinsztajn reaction. Under mild conditions, liquid analogues of conventional and commonly crystalline triarylamines are easily synthesized from readily available or accessible intermediates. Using a diverse selection of triarylamines, we explored the effects of siloxane group and substitution pattern on the physical properties of these materials, and we have demonstrated that relatively large molecular liquids with desirable electrochemical properties can be produced. The interactions between the strongly Lewis acidic catalyst used for this transformation, tris(pentafluorophenyl)borane (BCF), and the Lewis basic triarylamine substrates were studied. Through UV-vis-NIR and (19)F NMR spectroscopy, we have proposed that the catalyst undergoes a reversible redox reaction with the substrates to produce a charge transfer complex. The formation of this charge transfer complex is sensitive to the oxidation potential of the triarylamine and can greatly affect the kinetics of the Piers-Rubinsztajn reaction.     

基于联吡啶的π-共轭有机电致发光分子的合成和光学性质研究

利用Wittig-Horner方法合成了一系列新的基于联吡啶的π-共轭分子, 并用¹H NMR, ¹³C NMR、红外光谱、元素分析和MS进行了表征. 通过热重分析(TGA)测定结果表明所合成的化合物具有良好的热学稳定性; 化合物的光致发光(PL)最大发射峰在439～441 nm之间, 对应于蓝光区域.     

具有双极性端枝的3D结构化合物的合成及光学性能

通过Friedel-Crafts和Suzuki等反应合成了4种由核心和D-π-A双极性端基组成的3D结构类树枝状化合物, 并采用热重分析(TGA), 差热扫描量热分析和循环伏安等手段对其进行了表征. 结果表明, 该类化合物具有良好的热稳定性和电化学稳定性; 核的引入大大降低了端基D-π-A固态时分子间的聚集效应. 分子内电荷转移(ICT)导致化合物溶剂化效应的产生, 且其发光强度随着溶剂极性的变化而改变, 呈现正、 负溶致动力学现象.     

Synthesis and Characterization of Novel Polyamines Containing Different Substitute Groups Via Chemical Oxidative Polymerization

In this study, polymers of substitute aromatic amine compounds were synthesized by chemical oxidative polycondensation in aqueous alkaline medium using NaOCl as oxidant. The structures of synthesized compounds were confirmed by FT‐IR, UV‐Vis and NMR analyses. The characterizations of synthesized compounds were made by fluorescence, TG‐DTA, DSC, scanning electron microscopy (SEM) and Brunauer‐Emmett‐Teller (BET) surface area measurements. In addition, electrochemical and electrical conductivity values of compounds were carried out with cyclic voltammetry (CV) and four points probe technique measurements, respectively. Synthesized polymers viewed structural change, optical, electrochemical and thermal differences.     

Novel high phosphorus content phosphaphenanthrene-based efficient flame retardant additives for lithium-ion battery

The novel phosphate derivatives of phosphaphenanthrene with high-density phosphorus were synthesized and used as flame retardant additives for Li-ion batteries. The structures of compounds were characterized by ¹H NMR, ¹³C NMR, ³¹P NMR, FT-IR, and HR-MS. The excellent thermal stability of compounds was ascertained by thermogravimetric analysis and differential scanning calorimetry. The compounds were added to conventional electrolytes as flame retardant additives and evaluated their ionic conductivity, electrochemical stability, self-extinguishing properties, and combustion performance. The results showed that the compound containing higher phosphorus content has efficient flame retardant properties.     

Synthesis and characterization of N-carbazole end-capped oligofluorene-thiophenes

A series of novel N-carbazole end-capped oligofluorene-thiophenes with one, two, three, and four thiophene rings were synthesized using either palladium catalyzed cross-coupling reaction or nickel-catalyzed reductive dimerization. All the oligomers have been characterized by ¹H, ¹³C NMR, FTIR, UV-vis, PL spectroscopy and mass spectrometry. It has been demonstrated that the optical, thermal, and electrochemical properties of these materials can be tuned by varying the conjugation length of the oligothiophene segment. The terminal carbazole and fluorene moieties of the resulting materials are beneficial for their morphology, conjugation length, and solubility. These bright fluorescent, thermally and electrochemically stable compounds have potential applications as light-emitting and hole-transporting layers in organic light-emitting devices.     

基于芘并咪唑的电致发光材料的合成与表征

以芘和咪唑为基本构筑单元,利用"一锅法"合成了一系列芘并咪唑衍生物PyPI,PyTPAI,PyCzI和Pyd-CzI.采用质谱、核磁和元素分析等手段表征了化合物的结构.通过调节与芘并咪唑相连接的共轭基团的种类、大小和空间构型,实现对分子热学性质,分子轨道能级和光电性质的调控.进一步制备了有机电致发光器件,得到了较好的器件性能.