A mild, highly selective and remarkably easy procedure for deprotection of aromatic acetates using ammonium acetate as a neutral catalyst in aqueous medium

Ammonium acetate was found to catalyze efficiently the selective deprotection of aromatic acetates in the presence of various sensitive functionalities in aqueous methanol under neutral conditions at room temperature to yield the corresponding phenols in excellent yields. The method has been utilized for deprotection of acetates of several naturally occurring bioactive phenolic compounds and for preparation of venkatasin, a natural coumarino-lignan, from the anticancer compound cleomiscosin A.     

Electron capture detector response to low electron affinity aromatic hydrocarbons using positive ion stabilization and alkyl chloride sensitization

The electron capture detector (ECD) response to numerous aromatic hydrocarbons of low electron affinity (EA) is shown to be detrimentally affected by two processes which compete with and typically overwhelm the electron capture reactions of these molecules. It is shown that the effects of these two undesired reactions can be eliminated by the permanent addition of trimethylamine and one of several alkyl monochlorides to the detector make-up gas. These modifications of the detector gas result in greatly increased sensitivity, increased linearity, and increased reproducibility of response. A kinetic model for the ECD responses of low EA resonance capture molecules is developed which appears to explain these improvements.     

Synthesis of naphthyridines and phenanthrolines using catalysts based on transition and rare-earth metals

Liquid-phase condensation of 3-, 4-, and 8-aminoquinolines with aliphatic and aromatic aldehydes catalyzed by transition and rare-earth metal complexes is an efficient method for synthesis of substituted 1,7- and 1,6-naphthyridines and 1,10-phenanthrolines.Institute of Organic Chemistry, Ural Branch, Russian Academy of Sciences, 450054 Ufa; Eastern Scientific-Research Institute of Coal Chemistry, 620219 Sverdlovsk. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 5, pp. 1139–1148, May, 1992.     

基于氮化碳复合材料磁性固相萃取结合高效液相色谱法测定尿液中3种羟基多环芳烃

建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料，经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后，用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积（单次洗脱体积×洗脱次数）对萃取效率的影响。结合高效液相色谱-荧光分析，在0.25~250 μg/L范围内线性关系良好（相关系数r=0.999），3种羟基多环芳烃的检出限和定量限分别为0.08和0.25 μg/L，回收率为90.1%~102%，日内和日间精密度分别为1.5%~7.7%和2.2%~8.7%。该本方法简单、快速、高效，可用于尿液中羟基多环芳烃的分析。     

Catalytic degradation of polystyrene using HUSY catalysts

Summary The addition of carbon dioxide to phenyl glycidyl ether (PGE) was investigated in a semi-batch reactor using immobilized quaternary ammonium chloride catalysts. Five different catalysts were prepared with the following supports : (1) soluble poly(ST-<Emphasis Type=Italic>co</Emphasis>-VBC) [C1], (2) insoluble poly(ST-DVB-VBC) [C2], (3) macroporous poly(ST-DVB-VBC) [C3], (4) poly(ST-<Emphasis Type=Italic>co</Emphasis>-VBC)-MMT [C4] (5) modified MCM-41 [C5]. The addition of carbon dioxide to PGE can be considered as a pseudo-first order process with respect to the concentration of PGE. The pseudo-first order rate constant for the catalysts decreased in the series C1&gt;C3&gt;C2&gt;C4&gt;C5. The activation energy for C1 to C5 catalysts was 8.6, 20.9, 19.9, 23.9, and 26.8 kJ/mol, respectively. The immobilized catalysts can be reused in least 4 successive runs without any considerable loss of their initial reactivities.     

Synthesis and binding studies of new bis-calix[4]arenes containing aromatic and heteroaromatic units

A series of new bis-calix[4]arenes containing different aromatic and heteroaromatic moieties have been synthesized. The complexing behavior of these bis-calix[4]arenes have been studied towards different metal ions and it has been found that these bis-calix[4]arenes bind silver ions selectively over other metal ions. The complexation has been studied by liquid-liquid extraction and by NMR and IR spectroscopy.     

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．     

醛的自氧化振荡反应

1983年 Jensen 与 Roelofs 等报道了苯甲醛自氧化反应中出现的化学振荡现象。我们还观察到苯甲醛、取代苯甲醛和许多脂肪醛的自氧化振荡反应,实验方法与文献[3]相似。反应在具有电磁搅拌的恒温反应器中进行,以醋酸水溶液(冰醋酸与水的体积比为9∶1)和     

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。     

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%.