Novel poly(1H-benzo[g]indole)/TiO2 nanocomposites for high-performance electrochromic supercapacitor application

Poly(1H-benzo[g]indole) (PBIn)/TiO₂ nanocomposites with core-shell nanorod array morphology are successfully prepared via simply hydrothermal synthesis combined with electrochemical polymerization. The synergistic effect between PBIn and TiO₂ and the matched energy level distribution make PBIn/TiO₂ nanocomposites have a specific capacitance of 29.65 mF cm⁻². At the same time, it can reversibly change between light yellow and light green and show excellent cycling stability (86% retention after 3000 cycles). Thus, the electrochromic supercapacitor device (ESD) is also constructed based on PBIn/TiO₂ nanocomposite and poly(3,4-ethylenedioxythiophene). This ESD shows a good specific capacitance (13.2 mF cm⁻²) and high-coloring efficiency (487 cm² C⁻¹). In the charging and discharging stage, the color of ESD can reversibly change between yellow and dark blue. Thus, the accumulated energy state of the ESD can be simply judged by monitoring the color or transmittance value of the device. To verify the good energy storage and actual application, this ESD can light up the Light Emitting Diode (LED) after charging, which provides new possibilities for the application of intelligent supercapacitors in the future.     

E,E-1-(3＇-吲哚基)-5-取代苯基-1,4-戊二烯-3-酮化合物的合成及抗炎活性

戊二烯酮化合物;E;E-1-(3＇-吲哚基)-5-取代苯基-1;4-戊二烯-3-酮化合物的合成及抗炎活性     

Synthesis of N-Substituted Derivatives of 2-(4-Amino-2-methyl-1H-indol-3-yl)- and 2-(6-Amino-2-methyl-1H-indol-3-yl)acetic Acids

A method was developed for the production of indole compounds containing an amino group at positions 4 and 6 of the benzene ring on the basis of the indolization of the 3-acetylaminophenylhydrazone of ethyl levulinate. A series of derivatives of 2-(4-amino-2-methyl-1H-indol-3-yl)- and 2-(6-amino-2-methyl-1H-indol-3-yl)acetic acids at the 4- and 6-amino group were synthesized.     

Parallel Solid-Phase Synthesis of disubstituted 3-(1H-benzo[d]imidazol-2-yl)imidazolidine-2,4-diones and 3-(1H-benzo[d]imidazol-2-yl)-2-thioxoimidazolidin-4-ones

A multistep approach to construct novel 3-(1H-benzo[d]imidazol-2-yl)imidazolidine-2,4-diones and 3-(1H-benzo[d]imidazol-2-yl)-2-thioxoimidazolidin-4-ones from commercially available amino acids, amines, and carboxylic acids is described. Coupling of Fmoc-amino acid to resin-bound aminobenzimidazole provided following Fmoc elimination free amine. Treatment of the free amine with 1,1′-carbonyldiimidazole or 1,1′-thiocarbonyldiimidazole furnished the corresponding hydantoins and thiohydantoins via intramolecular cyclization. The desired aminobenzimidazole tethered hydantoins or thiohydantoins were isolated in good yields.     

Synthesis and Crystal Structure of (Z)-N-(2-(diethylamino)ethyl)-7-(5-fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamide Methanol Solvate

The crystal structure of a new compound (Z)-N-(2-(diethylamino)ethyl)-7-(5- fluoro-2-oxoindolin-3-ylidene)-2-methyl-4,5,6,7-tetrahydro-1H-indole-3-carboxamidemethanol solvate (C24H29FN4O2CH4O, Mr = 456.55) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 14.560(3), b = 7.3200(2), c = 22.233(4) , β = 101.78(3)°, V = 2319.7(8) 3 , Z = 4, Dc = 1.307 g/cm 3 , F(000) = 976, μ = 0.092 mm -1 , MoKa radiation (λ = 0.71073), R = 0.0604 and wR = 0.1644 for 4262 observed reflections with I > 2 (I). X-ray diffraction analysis reveals that the indole and pyrrole are almost coplanar. Intramolecular C-H···O and N-H···O hydrogen bonds together with π-π interactions are found in the structure.     

Synthesis of Cycloalk[b]indole Bearing Spiropiperidine Derivatives

The novel heterocyclic compounds that have cycloalk[b]indole moiety bearing spiropiperidinone and spiropiperidinedione ( 3a , 3b , 3c , 5a , 5b , 8a , 8b , and 10a ) were synthesized for the first time. The synthesis of spiropiperidinone and spiropiperidinedione structures was performed by a new method. These compounds are similar to sedative and hypnotic drugs such as methyprylon, glutethimide, and thalidomide.     

2-[3-(2-取代苯基)-1H-吡唑-1-基]-4,6-二甲氧基嘧啶类化合物的合成及除草活性研究

以邻羟基苯乙酮为起始原料,设计合成了22个新型的2-[3-(2-取代苯基)-1H-吡唑-1-基]-4,6-二甲氧基嘧啶类化合物,通过1H NMR,MS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除草活性.     

Synthesis of bis(indole)-1,2,4-triazinones

A facile method for the synthesis of para- and meta-substituted bis(indole)-1,2,4-triazinones is presented. Our approach to access these triazinones involves a cyclocondensation reaction between amidrazone and ketoester functionalities. The structures of these interesting compounds were established unambiguously by X-ray crystallography.     

1-[2-(2,4-二氯苯氧)乙酰基]-5-氨基-1H-吡唑衍生物的合成与生物活性

为寻求高效低毒的农药,设计、合成了一系列新的1-[2-(2,4-二氯苯氧)乙酰基]-5-氨基-1H-吡唑衍生物3a～3j和4a～4d.元素分析,1H NMR,IR和MS证实了它们的结构.初步的生物活性测试结果表明,在10 mg/L浓度下,化合物3a～3j和4a～4d对油菜的根茎均有很好的抑制作用,对油菜的根的抑制率为90.0%～98.7%;于100 mg/L浓度下,对稗草的根抑制率为84.0%～100%.     

基于3-(羧甲基)-7-甲基-2-丙基-3H-苯并[d]咪唑-5-羧酸的新型锌(Ⅱ)配位聚合物的合成及其晶体结构

以7-甲基-2-丙基-3H-苯并[d]咪唑-5-羧酸甲酯为原料,经还原反应和水解反应两步制得配体3-(羧甲基)-7-甲基-2-丙基-3H-苯并咪唑-5-羧酸(MZ);以Zn(NO_3)_2·6H_2O为锌源,MZ经配位反应合成一个新型的锌(Ⅱ)配合物{[Zn(MZ)_2]·2H_2O}_n(3),其结构经~1H NMR,FT-IR,X-射线单晶衍射和元素分析表征。3属单斜晶系,P2/c空间群,晶胞参数a=0.786 42(16)nm,b=1.072 1(2)nm,c=1.725 9(3)nm,α=γ=90°,β=93.63(3)°,V=1.452 2(5)nm3,D_c=1.482 g·cm~(-3),Z=2,R1=0.059 3,wR_2=0.141 5。     

2-溴-3-(1H-吲哚-3)-N-甲基马来酰亚胺的合成

以琥珀酰亚胺为起始原料,经过溴化、甲基化后再与吲哚溴化镁加成反应合成了2-溴-3-(1H-吲哚-3)-N-甲基马来酰亚胺,总收率44.8%,其结构经1H NMR和IR确证.     

1,2-双[2-甲基-5-(3,4-二氟苯基)噻吩-3-基]全氟环戊烯的合成

在冰浴条件下, 2-甲基噻吩(1)与液溴反应生成3,5-二溴-2-甲基噻吩(2); 在－78 ℃条件下, 硼酸三丁酯加入2, 得到2-甲基-3-溴-5-硼酸基噻吩(3); 3,4-二氟溴苯与3反应得到2-甲基-3-溴-5-(3,4-二氟苯基)噻吩(4); 在－78 ℃下全氟环戊烯与4反应, 得到一种新的二芳基乙烯类光致变色化合物1,2-双[2-甲基-5-(3,4-二氟苯基)噻吩-3-基]全氟环戊烯(DT-1). 用IR, NMR, MS和元素分析确定了化合物DT-1的结构, 并对该化合物的光致变色特性进行了初步研究.     

3-(噁唑-5-基)吲哚类天然产物生物活性及其衍生物的合成研究进展

3-(噁唑-5-基)吲哚类天然产物如Pimprinine,Streptochlorin等,广泛存在于海洋微生物中,因其具有多样的生物活性,在医药和农药领域中很有研究潜力.3-(噁唑-5-基)吲哚类天然产物的合成方法有很多研究报道,在吲哚结构上构建噁唑环是合成此类天然产物的关键.总结了已报道的3-(噁唑-5-基)吲哚类天然产物的生物活性,并对构建3-(噁唑-5-基)吲哚骨架的合成方法及部分主要反应机理进行了综述,探讨了3-(噁唑-5-基)吲哚类骨架作为一种优势活性结构在未来的应用前景.     

新型N-取代酰基-N-甲基-3-(1-萘氧基)-3-(2-噻吩基)丙胺的合成

为了得到具有更好抗抑郁活性的新型化合物,抗抑郁药度洛西汀通过N-酰化反应或N-烷基化反应与取代酰氯拼合,制得5个新型N-取代酰基-N-甲基-3-(1-萘氧基)-3-(2-噻吩基)丙胺,其结构经1H NMR,IR和MS表征.     

新型六氢吡啶-2,3-并吲哚化合物的合成及其抗肿瘤活性

以3-取代氧化吲哚与丙烯酸酯为原料,经Michael加成反应制得中间体--3-丙酸酯取代氧化吲哚（3a~3d）; 3a~3d与甲胺发生酰胺化反应制得3 丙酰胺取代氧化吲哚（4a~4d）; 4a~4d用氢化铝锂还原-环化,合成了4个六氢吡啶-2,3-并吲哚化合物(5a~5d）; 5a和5b用氢化铝锂还原合成了2个六氢吡啶-2,3-并吲哚化合物（6a和6b）, 5a～5d, 6a和6b均为新化合物,总产率42%～61%,其结构经¹H NMR, ¹³C NMR和HR-ESI-MS表征。采用MTT法研究了5a～5d, 6a和6b对人肺癌细胞（A549）,人前列腺（PC-3）和人白血病细胞（K562）的体外抗肿瘤活性。结果表明：5b对A549, PC 3和K562的抑制活性均较好,其IC₅₀分别为27.2μmol·L^-1, 37.5 μmol·L^-1和21.7 μmol·L^-1。     

1-(2-苯并呋喃酰基)愈创兰烃薁的合成

在路易斯酸作用下, 以氯乙酰氯为酰基化试剂, 对愈创兰烃薁进行了酰化反应研究, 将氯乙酰化产物与水杨醛在温和反应条件下进行缩合, 以较好的收率、高选择性地得到1-(2-苯并[b]呋喃酰基)兰烃薁类衍生物, 其结构经1H NMR, IR及元素分析等得以证实.     

新型吡唑硫代酰胺衍生物的合成

首次合成了7个新的5-(2-羟基-6-甲氧基苯基)-3-甲基-N-取代酰基-4,5-二氢吡唑-1-硫代酰胺衍生物,其结构经1H NMR,IR和元素分析表征。初步生物活性测试结果表明,部分化合物具有杀菌活性。     

达比加群酯中间体3-【【【2-{[(4-氰基苯基)氨基]甲基}-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸乙酯的合成

以对氨基苯腈为起始原料,经胺化反应制得N-(4-氰基苯基)甘氨酸(4);4与N-[3-氨基-4-(甲基氨基)苯甲酰基]-N-2-吡啶-β-丙氨酸乙酯(5)经酰胺化后经闭环反应,合成了达比加群酯的关键中间体——3-【【【2-{[(4-氰基苯基)氨基]甲基}-1-甲基-1H-苯并咪唑-5-基】羰基】(吡啶-2-基)氨基】丙酸乙酯,总收率79.6%,其结构经~1H NMR和ESI-MS确证。     

Synthesis and Crystal Structure of N-(2-(1-butyl-3-phenylureido)-1H-indol-3-yl)-N-(4-chlorophenyl)benzamide

<正>The title compound N-(2-(1-butyl-3-phenylureido)-1H-indol-3-yl)-N-(4-chloro- phenyl)- benzamide (C_(32)H_(29)ClN_4O_2, M_r = 537.04) was synthesized by a sequential Ugi four com- ponent condensation (4CC)/aza-Wittig/carbodiimide-mediated cyclization, and the structure was characterized by NMR, IR, MS, elemental analysis and X-ray single-crystal diffraction analysis. The crystal belongs to orthorhombic, space group P2_12_12_1 with a = 11.3663(9), b = 13.3248(10), c = 18.7887(15), V = 2845.6(4)~3, Z = 4, D_c = 1.254 mg/m3, μ = 0.170 mm~(-1), F(000) = 1128, the final R = 0.0538 and wR = 0.1187. X-ray analysis reveals that the new five-membered ring (C(14)-C(15)-N(2)-C(16)-C(21)) and the benzene ring (C(16)-C(21)) are nearly coplanar.