含咔唑和偶氮苯的乙炔衍生物的合成

采用Sonagashira偶联反应和N-烷基化反应合成了含有咔唑和偶氮苯的乙炔衍生物:3-乙炔基-9-(4-[4-(硝基)苯基偶氮苯]氧)亚丁基咔唑3.其结构通过IR,1H NMR,13C NMR,元素分析和X-射线单晶衍射法测定.标题化合物属单斜晶系,P21/c空间群;a=9.238(3),b=28.240(8),c...     

含二苯胺2,6-二咔唑基吡啶共轭化合物的合成

以咔唑,2,6-二溴吡啶和二苯胺为原料,经Ullmann和碘代反应合成了4个含二苯胺2,6-二咔唑基吡啶共轭化合物:3-二苯胺基-2,6二咔唑基吡啶,3,3’-二(二苯胺基)-2,6-二咔唑基吡啶,3,3’,6-三(二苯胺基)-2,6-二咔唑基吡啶和3,3’,6,6’-四(二苯胺基)-2,6-二咔唑基吡啶,其结构经1H NMR和IR确证。     

喹啉取代咔唑化合物的合成

以咔唑为原料,通过乙酰化反应合成了2-乙酰基咔唑(2)和3,6-二乙酰基咔唑(5);2和5分别与2-氨基二苯甲酮衍生物在酸催化下通过典型的Frledl(a)ender环化反应合成了一系列新的2-(4-取代苯基)喹啉咔唑和3,6-二(4-取代苯基)喹啉咔唑,其结构经1H NMR,IR和元素分析表征.     

N,N-二[4-(9H-9-咔唑基)苯基]-3,5-二溴苯胺的合成

以3,5-二溴苯胺,碘苯和咔唑为原料,经取代和Ullmann反应合成了一个新的含咔唑三苯胺化合物——N,N-二[4-(9H-9-咔唑基)苯基]-3,5-二溴苯胺,其结构经1H NMR,13C NMR和ESI-MS表征。     

新型联萘衍生物的合成及其光电性能

以咔唑和4,4’-二氨基-1,1’-联萘为初始原料,经重氮化反应、Ullmann反应、NBS亲电取代反应和Suzuki偶联反应,合成了两种新型空穴传输材料——4,4’-双[(9-对甲基苯基)-9H-3-咔唑基]-1,1’-联萘(4a)和4,4’-双[(9-对联苯基)-9H-3-咔唑基]-1,1’-联萘(4b),其结构经1H NMR和元素分析表征。研究了4a和4b在二氯甲烷中的UV和荧光性质。结果表明,4a和4b的最大发射波长分别为429 nm和427 nm。     

新型吡唑基咔唑衍生物的合成及其光学性质

以咔唑为原料,合成了一种新型的咔唑衍生物--9-丁基-3,6-二[3'-(5'-三氟甲基)吡唑基]咔唑(4),其结构经1H NMR,IR和MS表征.运用UV和单光子荧光光谱研究了中间体和4的光学性质,结果表明:4有望成为具有应用价值的发光材料.     

一种新型长共轭结构咔唑衍生物的合成及其光学性质

以咔唑、N,N-二甲基甲酰氨、溴丁烷和对甲基苯乙烯为原料,经Wittig反应和Heck反应合成了一种新型的长共轭结构的咔唑衍生物——3-[(对甲基苯乙烯基)苯乙烯基]-N-丁基咔唑(4),其结构经1H NMR,IR和元素分析表征。用UV-Vis和荧光光谱初步探讨了4的光学性质,结果表明,4具有良好的光学性质。     

偶氮基杯芳烃化合物的合成及其偶氮-醌腙互变异构性质

通过芳胺的重氮化-偶合反应合成了8个偶氮基杯芳烃化合物, 其结构经IR, 1H NMR, ESI-MS和元素分析表征. 通过UV-Vis, 1H NMR和IR考察了溶液pH值对所合成化合物5,11,17,23-四[(2-苯并噻唑基)偶氮基]-25,26,27,28-四羟基杯芳烃(3)和5,17-二[(1-萘基)偶氮基]-25,26,27,28-四羟基杯芳烃(4)的偶氮-醌腙互变异构的影响. 结果表明, 随着溶液pH值增加, 醌腙体在偶氮-醌腙互变异构平衡中的比例增加, 当pH≥10时, 几乎全部转变为醌腙体. 特别当溶液pH=-1时, 化合物4可以形成一种大的共轭体系, 使其λmax由477 nm红移至545 nm.     

新型三唑基咔唑衍生物的合成及其光学性质

合成了一种新型的三唑基咔唑衍生物--3,6-二(1,2,4-三唑)-N-己基咔唑(4),其结构经1H NMR, IR和MS表征.利用UV,单光子荧光光谱和固体荧光光谱研究了4的线性光学性质,结果表明4有望成为具有应用价值的发光材料.     

新型含取代乙烯基香豆素衍生物的合成及其光学性能

利用Perkin反应和Wittig反应设计并合成了两个新型的香豆素衍生物——3-(4’-溴苯基)-7-(N-辛基-3’-溴咔唑-6’-乙烯基)香豆素(6a)和3-(4’-溴苯基)-7-(4’-甲氧基苯基-1’-乙烯基)香豆素(6b),其结构经UV,1H NMR,IR,MS和荧光光谱表征。研究结果表明,6a和6b具有荧光强度大和Stokes位移(分别为115 nm和122 nm)大的特点。     

含酰基吡唑啉酮和咔唑光功能基元的新型席夫碱的合成

以苯肼、乙酰乙酸乙酯和咔唑为原料,合成了一种含酰基吡唑啉酮和咔唑双光功能基元的新型席夫碱———1-苯基-3-甲基-4-苯甲酰基-吡唑啉酮-5缩N-对氨基苄基咔唑(6),其结构经1H NMR和IR确证;采用UV-vis对其电子结构进行了初步研究,与酰基吡唑啉酮或咔唑功能基元相比,6表现出特殊的电子结构。     

咔唑衍生物的固相合成及其双光子吸收和光存储应用

以N-乙基咔唑为原料,通过室温固相化学反应改进合成了2种双光子吸收材料(咔唑类衍生物2, 8-二[2'-(吡啶-4"-基)乙烯基]-5-乙基咔唑(L1),2, 8-二[2'-(吡啶-2"-基)乙烯基]-5-乙基咔唑(L2),其结构经¹H NMR,IR和MS确证,利用Z-扫描技术,测试了其纳秒下的双光子吸收截面为6 210和5 590 GM (1 GM = 1 ´ 10 ^-50 cm ⁴ · s · photon ^-1),用820 nm的飞秒单脉冲激光作为写入激光对存储介质进行双光子光漂白,对其作为三维光存储材料作了初步的探索。     

N,N’-二苯基-N,N’-二(9,9-二甲基芴-2-基)-9-己基-(4,4’-二胺基苯基)咔唑的合成方法及表征

以2,7-二溴咔唑为原料经过N-烷基化、Suzuki偶联反应、Buchwald-Hartwig偶联反应合成了有机发光二极管(OLED)空穴传输材料N,N’-二苯基-N,N’-二(9,9-二甲基芴-2-基)-9-己基-(4,4’-二胺基苯基)咔唑,利用NMR、IR和熔点等分析方法对产物结构进行了表征,并通过TG、UV-Vis及荧光光谱研究了物质的热稳定性和光学性能。     

还原温度对氧化铝负载的磷化钨催化剂咔唑加氢脱氮活性影响(英）

采用共浸渍和程序升温还原的方法,在不同的温度下氢气还原4h合成了负载量为30%（以WO3计）的WP/γ-Al2O3催化剂。对合成的催化剂进行了XRD、BET、TG和31P MAS NMR表征。在3.0MPa和633K的反应条件下,对催化剂的咔唑加氢脱氮（HDN）活性进行了评价。结果表明,当还原温度超过1023K时活性组分WP在载体表面发生聚集。当催化剂还原温度为923K时,在化学位移为2.4×10-5只能检测到与磷酸盐对应的特征峰;当催化剂还原温度为1023K和低旋转频率时,在化学位移为2.55×10-4处检测到与活性组分WP对应的特征衍射峰,当高旋转频率时,在化学位移为处6.88×10-4处检测到一个特征峰,该特征峰可能与载体和活性组分之间存在的强相互作用而产生的类似—Al—O—W—P结构的物种有关,这对应与XRD谱图中在40.44°存在的衍射峰。TG结果表明,随还原温度的提高,催化剂前体的磷化程度增加。923K合成的催化剂具有相对最高的咔唑HDN活性,其咔唑HDN转化率达到79%。催化剂咔唑HDN途径有三条：比较低的直接氢解脱氮选择性和比较高的加氢脱氮选择性（一个苯环先饱和然后脱氮,两个苯环饱和然后再脱氮）,其中第三条途径,即两个苯环饱和再脱氮为主要途径。     

Synthesis and characterization of a trefoil-shaped liquid crystal based on 1,3,5-triazine with carbazole groups

A trefoil-shaped liquid crystal containing an aromatic hetero-nucleus has been synthesized by the reaction of cyanuric chloride with 3,6-didecanoyl carbazole (DDC). The molecular structure was characterized by ¹H NMR and ¹³C NMR spectroscopy, mass spectroscopy and elemental analysis. The core consists of 1,3,5-triazine directly linked to three carbazole groups. The trefoil-shaped conformation is suggested by molecular modelling. The mesophase was investigated using DSC, X-ray diffraction and polarizing optical microscopy. The X-ray diffraction pattern of a sample cooled slowly from the isotropic state showed sharp peaks in the small angle and wide angle regions implying the existence of a columnar phase with interand intra-columnar ordering. An unusual reticular texture similar to a cholesteric texture was observed.     

Synthesis and characterization of a trefoil-shaped liquid crystal based on 1,3,5-triazine with carbazole groups

A trefoil-shaped liquid crystal containing an aromatic hetero-nucleus has been synthesized by the reaction of cyanuric chloride with 3,6-didecanoyl carbazole (DDC). The molecular structure was characterized by ¹H NMR and ¹³C NMR spectroscopy, mass spectroscopy and elemental analysis. The core consists of 1,3,5-triazine directly linked to three carbazole groups. The trefoil-shaped conformation is suggested by molecular modelling. The mesophase was investigated using DSC, X-ray diffraction and polarizing optical microscopy. The X-ray diffraction pattern of a sample cooled slowly from the isotropic state showed sharp peaks in the small angle and wide angle regions implying the existence of a columnar phase with interand intra-columnar ordering. An unusual reticular texture similar to a cholesteric texture was observed.     

N-乙基咔唑的绿色高效合成

以咔唑为原料,碳酸二乙酯为烷基化试剂,碳酸铯和三乙基苄基氯化铵为共催化剂,经烷基化反应绿色合成了N-乙基咔唑,其结构经¹H NMR和HR-ESI-MS确证。在最佳反应条件［咔唑200 mmol,碳酸二乙酯1.2 eq.,碳酸铯（0.05 eq.）和三乙基苄基氯化铵（0.05 eq.）为催化体系,于180 ℃反应3 h］下,产率99%。     

First total synthesis of eudistalbin A

<正>Eudistalbin A was isolated from marine tunicate eudistoma album and possess cytotoxic activity(ED_(50)3.2μg/mL) in vitro against the growth of KB human buccal carinoma cells.The synthetic eudistalbin A showed potent inhibitory activity against the breast carcinoma cell line MDA-231 with an IC_(50) value of 2.1μmol/L using the metabolic assay MTT.All structures of new compounds were confirmed by ~1H NMR,~(13)C NMR,HRMS and optical rotation.     

AπDπA型咔唑衍生物三阶光学非线性的Z-扫描研究

合成了6个新型AπDπA型3,6-二取代咔唑多极生色分子, 用红外光谱、核磁共振等对其结构进行了表征. 用Z-扫描方法研究了这些分子的三阶非线性光学性质. 实验结果表明, 这些分子具有较大的三阶极化率, 延长共轭链长度, 增加电子受体强度, 引入芳香杂环, 都能增强分子内电荷转移, 这种效应增加了分子的跃迁矩, 使三阶极化率增大.     

Synthesis and characterization of highly stable blue‐light‐emitting hyperbranched conjugated polymers

Polyfluorene homopolymer ( P1 ) and its carbazole derivatives ( P2 – P4 ) have been prepared with good yield by Suzuki coupling polymerization. P2 is an alternating copolymer based on fluorene and carbazole; P3 is a hyperbranched polymer with carbazole derivative as the core and polyfluorene as the long arms; P4 is a hyperbranched polymer with carbazole derivative as the core and the alternating fluorene and carbazole as the long arms. These polymers show highly thermal stability, and their structures and physical properties are studied using gel permeation chromatography, ¹H NMR, ¹³C NMR, elemental analysis, Fourier transform infrared spectroscopy, thermogravimetry, UV–vis absorption, photoluminescence, and cyclic voltammetry (CV). The influence of the incorporation of carbazole and the hyperbranched structures on the thermal, electrochemical, and electroluminescent properties has been investigated. Both carbazole addition and the hyperbranched structure increase the thermal and photoluminescent stability. The CV shows an increase of the HOMO energy levels for the derivatives, compared with polyfluorene homopolymer ( P1 ). The EL devices fabricated by these polymers exhibit pure blue‐light‐emitting with negligible low‐energy emission bands, indicating that the hyperbranched structure has a strong effect on the PLED characteristics. The results imply that incorporating carbazole into polyfluorene to form a hyperbranched structure is an efficient way to obtain highly stable blue‐light‐emitting conjugated polymers, and it is possible to adjust the property of light‐emitting polymers by the amount of carbazole derivative incorporated into the polymers. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 790–802, 2008