微波辐射下2-氨基-7-甲基-4-芳基-5-氧代-4H,5H-吡喃并[4,3-b]吡喃-3-腈的一步合成

芳醛、丙二腈与6-甲基-4-羟基-2-吡喃酮在微波辐射下, 一步反应得到一系列2-氨基-7-甲基-4-芳基-5-氧代-4H,5H-吡喃并[4,3-b]吡喃-3-腈, 该反应时间短、产率较高、环境友好、后处理简单. 产物的结构经红外光谱、核磁共振谱和元素分析表征, 产物4g的结构经单晶X射线衍射进一步确证; 并对反应过程提出了可能的机理.     

条带织构装饰技术观察含T─型液晶基元的热致性聚芳酯液晶态的向错

采用条带织构装饰新技术研究了含Ｔ─型液晶基元的热致性聚芳酯液晶态的向错形态．经过培养的液晶样品无需剪切，淬火后便可呈现出围绕向错点取向排列的条带织构，而条带织构长轴的垂直方向正代表了液晶基元的指向矢方向，这样，在普通偏光显微镜下就能直接观察到这些条带织构装饰的强度Ｓ＝±１／２和Ｓ＝±１的向错，并观察到Ｓ＝－３／２的高强度向错和闭环状的反转壁．     

纳米多孔双金属氧化物在镍钛合金纤维上的原位生长及其对多环芳烃的选择性固相微萃取

采用阳极氧化法在镍钛合金(NiTi)纤维上原位生长了双金属氧化物纳米孔(NiTiONPs)涂层,通过扫描电镜(SEM)和能谱(EDS)考察了电解质组成和电压对形貌的影响。将NiTiONPs涂层的NiTi纤维与高效液相色谱-紫外检测器联用,研究了4种典型芳香分析物的萃取性能。结果表明,富含TiO2的NiTiONPs涂层对多环芳烃(PAHs)具有良好的萃取效率,尤其对苯并[a]芘的萃取选择性优于市售聚二甲基硅氧烷纤维和聚丙烯酸酯纤维。在优化条件下,PAHs的线性范围为0.05~200μg/L,相关系数均大于0.999,检出限为0.012~0.134μg/L。对单支纤维日内和日间分析的相对标准偏差(RSDs)分别为4.0%~5.5%和6.0%~6.8%,使用分批组装的5支纤维分析的RSDs为6.4%~7.6%。实际水样分析的加标回收率为84.5%~111.5%。所制备NiTi纤维至少可重复使用250次以上,重现性好。     

SNAr reactions of β-substituted porphyrins and the synthesis of meso substituted tetrabenzoporphyrins

Reaction of 2,3,7,8,12,13,17,18-octaethylporphyrin with LiR reagents containing functional groups readily yields meso substituted derivatives suitable for further transformations with residues such as -p-C₆H₅Br, -p-C₆H₅-CCH, -p-C₆H₅-NH₂ or -(CH₂)₃-CHCH₂. Similar reactions of tetrabenzoporphyrin with alkyllithium reagents afforded the first entry into meso mono- and dialkylsubstituted tetrabenzoporphyrins while reaction of bicyclo[2.2.2]oct-type masked isoindole precursors with LiR followed by in situ retro-Diels-Alder reaction also afforded the 5-phenyl and 5,10-diphenyltetrabenzoporphyrins in high purity.     

Electrochemical Amination in the System Ti(IV)–NH2OH–C6H6: The Efficiency of the Process in a Sulfuric Acid Solution Containing an Organic Solvent

Electrolysis of the system Ti(IV)–NH₂OH–C₆H₆ in an 11 M H₂SO₄ solution shows that using an organic solvent (acetic acid, acetonitrile) during cathodically initiated amination of aromatic substrates permits the production of aromatic amines with the overall yield by hydroxylamine reaching 91%. Due to a chain mechanism of radical substitution, the benzene amination in electrolytes containing 5 M CH₃COOH and 5.5 M CH₃CN terminates largely upon consuming 70–75 and 50–55% of the charge required theoretically for a one-electron process. The maximum efficiency of electrochemical amination is observed at low hydroxylamine conversions and the overall current efficiency for mono- and disubstituted products of the benzene amination may exceed in these conditions 750%.     

Hydrogen Effect on Coke Removal and Catalytic Performance in Pre-Carburization and Methane Dehydro-Aromatization Reaction on Mo/HZSM-5

1. Introduction As an effective utilization of methane, the methane dehydro-aromatization was focused in the last decade [1-28]. Over the Mo/HZSM-5 bi- functional catalyst at high reaction temperature, methane can be converted into light aromatics (ben- zene and naphthalene) and hydrogen. Mo active species can activate the C—H bond of methane; and HZSM-5 supplies the acid sites for the oligomeriza- tion and cyclization of hydrocarbons to form aromat- ics, and suppresses the deeper condens…     

硼化合物的研究——Ⅴ.氢硼酸π-芳烃-π-环戊二烯基铁的合成和性质

本文研究了氢硼酸根(B_(12)H_(12)~(2-)、B_(10)H_(10)~(1-)、B_(11)H_(14)~-)和π-芳烃-π-环戊二烯基铁阳离子的反应,合成了36个氢硼酸π-芳烃-π-环戊二烯基铁化合物。通过元素分析和红外光谱测定确定了化合物的组成。部份化合物还作了~1H NMR鉴定。对化合物的性质,包括它们的热行为,进行了较详细的研究。DTA仪测得的结果表明,(1)当阳离子相同时,化合物的热稳定性的顺序为:[ArFeC_5H_5]_2B_(12)H_(12)>[ArFeC_5H_5]_2B_(10)H_(10)>[ArFeC_5H_5]B_(11)H_(14);(2)当氢硼酸根相同时,其热稳定性受芳环上取代基的影响。     

Reactions of (η6-Arene)tricarbonylchromium Complexes: Hydrogenation,Nitration, and Bromination

In this study, we explore the reactions of coordinated arenes, e.g., hydrogenation, nitration, and bromination, to prepare compounds which are not accessible from conventional organic synthesis. The reaction products formed from reactions with the coordinated and the uncoordinated arenes are compared. The polycyclic aromatic hydrocarbons (PAHs) employed for this study include phenanthrene, methyl- and acetyl-phenanthrene, and benz[a]anthracene (BA), The tricarbonylchromium group demonstrated various characteristics which influence the reactions in this work, such as an electronic effect to deactivate hydrogenation, a steric effect to exhibit, highly positional selective nitration, and a free radical mechanism to direct bromine to attack at the ring coordinated to tricarbonylchromium.     

Synthesis of triphenylene derivatives by Pd-catalyzed Suzuki coupling/intramolecular CH activation between arylboronic acids and dibromobiphenyls

An efficient and regioselective synthesis of functionalized triphenylenes via palladium-catalyzed Suzuki-Miyaura coupling and subsequent intramolecular CH activation between arylboronic acids and dibromobiphenyls was developed. This methodology showed excellent atomic economy and regiospecificity as well as synthetic feasibility of unsymmetrical triphenylenes.     

Rigid aromatic fractal polyamides

The preparation of rigid aromatic, highly branched polyamides is described. Owing to the method of preparation and the chosen ratio of difunctional to trifunctional monomers, these entities are highly porous and not dendrimeric in nature. They better conform with the fractal model and are therefore called fractal polyamides (FPs). The effects of variations in the polymerization procedure, in total monomer concentration, in the ratio of amine to carboxyl groups and in the duration of the polycondensation reaction are investigated. Some characterization was performed and the results are presented and briefly discussed.