Synthesis,Properties, and Special Features of the Fragmentation under Electron Impact of N-Substituted Nicotinoyl Ureas

A convenient preparative synthetic route has been developed and N’-substituted nicotinoyl ureas have been obtained for the first time. Possible directions have been studied for their fragmentation under electron impact.__________Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 705–712, May, 2005.     

Ultrasound-accelerated Synthesis of 1,4-Dihydropyridines in an Ionic Liquid

Summary. Hantzsch 1,4-dihydropyridine compounds were synthesized efficiently in high yields at room temperature within short times in 1,1,3,3-N,N,N′,N′-tetramethylguanidinium trifluoroacetate as ionic liquid using ultrasound irradiation. The ionic liquid can be recovered conveniently and reused efficiently.     

离子液体中12-苯甲酰基脱氢松香酸甲酯的合成

以离子液体[bmim]Br/AlCl3作为绿色反应介质,通过脱氢松香酸甲酯芳环上的Friedel-Crafts酰基化反应,合成了12-苯甲酰基脱氢松香酸甲酯,最佳合成条件为:脱氧松香酸甲酯、[bmim]Br、AlCl3、苯甲酰氯的摩尔比1:4:8:8,反应温度40℃,反应时间2h.用IR、MS、NMR和元素分析等方法对目标产物进行了分析和表征.结果表明,该合成方法具有反应条件温和、反应时间短及环境友好等优点.     

微波辅助离子液体法在液相合成中的应用

作为一种新型的绿色化学合成方法,微波辅助离子液体法融合了离子液体与微波加热法的优点,具有合成快速、操作简便、产率高,绿色环保等特点,在液相合成方面体现出明显的优势。本文综述了离子液体作为微波吸收剂在液相有机合成、无机纳米材料合成方面的研究进展,对比分析了微波辅助离子液体法同多种传统方法的应用效果,阐明了该方法的优势,并展望该领域今后的发展方向。     

双功能离子液体的合成及二氧化碳捕集性能

采用两步法合成了新型功能化离子液体1-甲氧基乙基-3-甲基咪唑甘氨酸([C_3O_1mim][Gly]),并研究了其对CO_2的吸收性能.利用核磁共振、红外光谱及热重分析等手段进行表征,验证了该离子液体的结构,且发现其具有较高的热稳定性.对比单乙醇胺(MEA),考察了[C_3O_1mim][Gly]在不同温度下对CO_2的捕集能力,结果表明,[C_3O_1mim][Gly]在40℃下的吸收容量可达1.26 mol CO_2/mol IL,远高于MEA,这表明[C_3O_1mim][Gly]对CO_2具有良好的吸收能力,吸收容量随着温度升高而降低.该离子液体同时具有良好的循环稳定性,进行5次吸收解吸操作后仍可保持较高的CO_2吸收量.对该离子液体吸收CO_2进行了动力学研究,结果表明,Pseudo-second-order模型能够较好地描述该吸收过程.     

碱性离子液体催化合成三羟甲基丙烷

以碱性离子液体为催化剂, 构建了一种新型、高效的合成三羟甲基丙烷(TMP)的方法. 系统考察了催化剂类型、催化剂用量、反应温度、反应时间、甲醛与正丁醛用量比等因素对三羟甲基丙烷分离收率的影响. 研究结果表明: 碱性离子液体的催化性能与其碱强度息息相关, 碱性越强、催化活性越高. 最优条件下, 经离子液体[bmim]OH催化后, 可得到84%的TMP分离收率, 这一结果优于传统的有机无机碱催化体系且成功规避了传统碱催化合成TMP过程中繁琐的除盐过程、降低了过程能耗. 此外, 离子液体催化剂和未反应的丁醛均表现了良好的重复使用性能.     

Sequential [2+2] Photocycloaddition and Rearrangement to Substituted Cyclopentanone. A formal Synthesis of Planococcyl Acetate

An extremely short synthesis of 2,2-dimethyl-3-hydroxymethyl cyclopentanone 2 (R¹ = R² = Me), an advanced intermediate in the synthesis of the pheromone planococcyl acetate 3, is described.     

Efficient and Green Synthesis of N‐aryl Pyrroles Catalyzed by Ionic Liquid [H‐NMP][HSO4] in Water at Room Temperature

A suitable and efficient method for the synthesis of N‐aryl pyrroles by using 2,5‐dimethoxy tetrahydrofuran and several primary aromatic amines in the presence of the catalytic amount of [H‐NMP][HSO₄] under room temperature was described. This method has the advantages such as; easy reaction workup, absolutely separated of catalyst from the reaction mixture and smoothly recyclability of catalyst. In this reaction, N‐substituted pyrroles were obtained as desired products in excellent yields and short reaction times via green and one‐pot procedure.     

Amberlyst‐15‐Catalyzed Novel Synthesis of Quinoline Derivatives in Ionic Liquid

In recent years, ionic liquids have attracted much attention as useful synthetic solvents. Compared with classical molecular solvents, the ionic liquids are environmentally benign reaction media. A variety of quinoline derivatives have been synthesized under ionic liquid conditions using Amberlyst‐15 as catalyst.     

离子液体体系中离子型锰卟啉对苯乙烯的催化氧化

以单氧给体乙酰碘苯[PhI(OAc)2]为氧源, 在无需轴向配体和有机溶剂的参与下, 离子型锰卟啉[MnⅢ(BF4)T(N-Me-4-Py)P][BF4]4和离子液体 [BMIM]BF4组成的多元离子液体体系, 在温和的反应条件下对苯乙烯的催化氧化表现出较高的活性(87%)和环氧苯乙烷选择性(90％), 并且有较好的底物普适性. 构筑的锰卟啉多元离子液体体系可以一定程度上抑制卟啉聚合和氧化降解等反应.     

Synthesis of Thioglycosides in Room Temperature Ionic Liquid

An eco-friendly reaction for the preparation of thioglycosides has been developed using an ionic liquid as the solvent. Thioglycosides were obtained in excellent yields on treatment of per-O-acetylated sugar derivatives with thiols in the presence of boron trifluoride diethyl etherate in [Bmim][BF₄] as solvent at 20°C. Supplemental materials are available for this article. Go to the publisher's online edition of Journal of Carbohydrate Chemistry to view the free supplemental file.     

室温离子液体中合成方钠石的研究

本文以离子液体为溶剂, 在常压下采用离子液体热合成方法合成了方钠石分子筛.     

以离子液体为结构导向剂合成有序超微孔二氧化硅

在酸性条件下, 以1-十六烷基-3-甲基溴化咪唑为表面活性剂合成了具有有序超微孔结构的二氧化硅材料, 所合成的材料具有较高的比表面积和二维六方有序的孔结构, 样品的孔径尺寸为1.8 nm.     

塑晶基离子液体合成及其电化学性能

通过简单、易于工业化的重结晶方法制备了高纯1-甲基-1-乙基吡咯烷鎓双(三氟甲基磺酰)亚胺盐(P₁₂TFSI)塑晶化合物. 在此化合物中加入30% (摩尔分数, x)双(氟磺酰)亚胺锂(LiFSI)后, 得到P₁₂TFSI/LiFSI 塑晶基离子液体. 采用循环伏安法、恒电压极化法及恒电流充放电法等电化学方法考察了该离子液体的电化学窗口、铝箔集流体的腐蚀性及电池性能. 结果表明, 该离子液体电解质具有5.00 V的电化学窗口, 室温离子电导率达到0.92 mS·cm^-1, 且不腐蚀Al 集流体. 以该塑晶离子液体作为电解液组装的实验电池LiCoO₂/Li 表现出良好的充放电特性及循环性能, 在较低倍率下能够和使用碳酸酯类电解液组装的实验电池的性能相媲美. 在4.50 V高电压下, 循环20周后, 容量仍能保持在175 mAh·g^-1, 容量保持率为95.1%. 这些结果说明该离子液体在高性能锂二次电池中具有良好的应用前景.     

An Efficient Synthesis of Pyrazolo[3,4-b]pyridine Derivatives in Ionic Liquid

A series of 3-methyl-1,4,6-triaryl-1H-pyrazolo[3,4-b]pyridines was synthesized via the reaction of 3-methyl-1-phenyl-1H-pyrazol-5-amine and α,β-unsaturated ketones in ionic liquid without any catalyst. This protocol has the advantages of easier work-up, milder reaction conditions, high yields and environmentally benign procedure.     

离子液体改性的气相色谱固定相研究

合成了哑铃型离子液体, 并将FFAP与其按2∶1的质量比混合涂渍交联在石英管内壁, 柱效为3500 p/m, 极性为435.2, 比FFAP柱的极性明显降低. 但由混配的固定相制成的色谱柱对极性和弱极性物质的选择性都优于FFAP柱. 此外, 该固定相对芳香位置异构体、羧酸、烷烃、醇类、酯类及多环芳烃混合物等均具有较好的分离选择性.     

A New Simple and Efficient Synthesis of N-Aryl Phthalimides in Ionic Liquid [bmim][PF6]

Abstract

The room temperature ionic liquid [bmim][PF₆], namely 1-butyl-3-methyl-imidazolium hexafluorophosphate, is used as an alternative solvent to classic solvents for the synthesis of a series of N-aryl phthalimides in good to excellent yields.     

聚噻吩在离子液体中的电化学合成研究

Polythiophene（PTh）films were prepared by the direct electropolymerization of thiophene in the ionic liquid,1-butyl-3-methylimidazolium hexafluorophosphate（BMIM）PF6 . The structure and morphology of PTh films were characterized by means of the FT-IR spectrum and the scanning electron microscopy（ SEM）. The electrical and electrochemical properties of PTh films were examined with the UV-Vis spectrum,cyclic voltammetry（CV） and four-probe method. The results showed that when the potential for electropolymerization was controlled between +1.7 and +1.9 V（vs. Ag/AgCl）,very homogeneous PTh films could be prepared in the ionic liquid （BMIM）PF6 used as solvent and electrolyte. The de-doping（reduction）and re-doping（re-oxidation）of the PTh film prepared in ionic liquid are reversible and stable,and the conductivity of PTh films is 0.01-0.1 S/cm.     

聚硅氧烷键合离子液体的合成及色谱性能

提出了一种基于聚硅氧烷键合离子液体(PSOIL)的气相色谱固定相的方法, 即首先合成γ-氯丙基聚硅氧烷, 然后通过氯丙基与甲基咪唑的反应合成了聚硅氧烷负载的离子液体, 并对其色谱性能及分离选择性进行了评价.     

Facile Synthesis of Cyclodextrin Functionalized Reduced Graphite Oxide with the Aid of Ionic Liquid for Simultaneous Determination of Guanine and Adenine

Here, a facile reduction approach for synthesis of β‐cyclodextrin functionalized reduced graphite oxide with the aid of ionic liquid (βCD/IRGO) was reported. This strategy relies on the simple mixing of pre‐pared aqueous βCD/GO with ionic liquid (IL) at high temperatures, which can bring about a well dispersed βCD/RGO in the utilized IL (βCD/IRGO) with a synchronous evaporation of water. The as‐prepared βCD/IRGO product can be stably re‐dispersed in water (up to 1.0 mg/mL) after washed and dried. And the presented βCD/IRGO composites possess high supramolecular recognition capability and good conductivity for realizing enhanced electrochemical response towards simultaneous detection of guanine and adenine compared with other βCD/carbon (RGO or carbon nanotube) based composites. In the presence of one of analysts, the linear response ranges is 0.03–10.0 μM for guanine and 0.02–7.0 μM for adenine, respectively, with detection limit of 0.01 μM for both guanine and adenine (S/N=3). This ease of making the βCD/IRGO composite will open up possibilities of its diversifier applications.