UV/Vis-spektroskopische Untersuchungen an Cyclosilanderivaten

UV/Vis-spectra of Cyclosilanes (SiX ₂) _n withX=Cl, Br, I, OMe andn=4, 5, 6 are recorded and interpreted qualitatively. The spectra exhibit increasing influence of the substituents on the Si-Si-bond system within the rings in the order Cl OMe Br I. At the low energy side of the spectra weak absorption bands, possibly due to intramolecular charge transfer transitions, appear. The strong inductive effect of the electronegative substituents is documented by a marked increase of the first IP's compared to permethylcyclosilanes.

     

微波干法催化芳香醛与绕丹宁及N-苯基绕丹宁的缩合反应

利用微波辐射和固体碱性载体试剂催化绕丹宁及N-苯基绕丹宁和芳香醛的缩合反应合成了14个绕丹宁衍生物并研究了影响反应的因素。     

2-取代吡啶半菁染料的无溶剂微波合成及光谱性质的理论研究

在微波促进无溶剂条件下, 由N-甲基-2-甲基吡啶碘盐与取代芳香醛在哌啶作用下合成了一系列2-取代的吡啶半菁染料, 产物结构由元素分析, ¹H NMR, MS, IR, UV得到确认. 该方法操作简便, 收率高. 在此基础上, 对N-甲 基-2-(p-N,N-二甲氨基-苯乙烯基)吡啶半菁染料的光谱性质进行了理论计算.     

光固化环氧丙烯酸酯/SiO2杂化材料的研究

用FTIR、SEM、DSC和TGA表征了光固化环氧丙烯酸酯／SiO2杂化材料[(EA-TMSPM)／SiO2]，研究了盐酸、γ-甲基丙烯酰氧丙基三甲氧基硅烷(TMSPM)和无机物浓度对(EA-TMSPM)／SiO2结构与性能的影响。结果表明，无机物浓度高的(EA-TMSPM)／SiO2杂化体系中SiO2粒子尺寸略大于无机物浓度低的体系；盐酸和无机物浓度的增加，都可以增强杂化材料的耐磨性。     

手性芳酰胺类分子钳的设计与微波合成

以间苯二甲酸为隔离基, 酰胺键桥联L-氨基酸甲酯构成手臂, 在微波辐射下合成了具有不同手性中心和裂穴的新型手性芳酰胺类分子钳. 结构均经¹H NMR, IR及元素分析确证, 并考察了其对芳香胺类化合物和D/L-氨基酸甲酯的识别性能. 初步研究表明, 这类分子钳受体不仅对中性小分子具有优良的识别性能, 其结合常数(K_a)可达2.66×10³ L•mol^－1, 而且对D/L-氨基酸甲酯亦具有良好的手性识别能力.     

Developing an on-line derivatization of FAs by microwave irradiation coupled to HPLC separation with UV detection

The development of analytical methods for routine simultaneous identification and quantification of carboxylic fatty acids (CFAs) are required in different fields, such as, pharmaceutical cosmetics, food products and formulations of water–microemulsion–oil systems. Determination of CFAs has been developed mainly by gas chromatography (GC). As an alternative to GC, liquid chromatography (LC) has better sensitivity and selectivity. However, most CFAs show no useful absorption in ultraviolet–violet (UV–Vis) region, one of the more used detection technique in high-performance liquid chromatography (HPLC). In order to allow the use of UV–Vis detection, the use of pre-column derivatization has been reported to increase sensitivity and selectivity. Therefore, establishment of a simpler and faster on-line method with complete separation is needed for the screening of large numbers of samples. 2,4-Dinitrophenylhydrazine (2,4-DNPH.), benzoil chloride (BC), and phenylhydrazine (PH) were used for derivatization of different FAs by microwaves radiation (MW). After the on-line derivatization, products were separated and quantified by HPLC. Reactor coil was placed inside of microwaves oven at 450 W. Parameters as flow, amount of reagents, irradiation time, and chromatographic conditions were optimized. The continuous analysis using the MW–HPLC–UV system provided high sensitivity and reduced both the amount of reagent used and the analysis times. This proposed method can be used for the routine analysis of FAs contained in water–microemulsion–oil systems, to quantify the total acid fraction in each phase.     

微波辐照下无皂阳离子聚(St-MMA)高分子纳米粒子的制备和表征

讨论了微波辐照下 ,以丙酮 水为分散介质 ,利用阳离子型自由基引发剂偶氮二异丁基脒盐酸盐(AIBA)引发苯乙烯 (St)和甲基丙烯酸甲酯 (MMA)共聚 ,合成出表面带正电荷的P(St MMA)共聚物纳米粒子 ,考察了丙酮用量、单体和引发剂浓度对纳米粒子粒径、粒径分布和乳液稳定性的影响 .结果表明 ,丙酮 水的体积比由 0增加到 1 2 6∶1时 ,粒子的平均水化半径从 12 2 2 1nm降低到 2 4 6 8nm ,粒径分布变宽 ,乳液抗电解质稳定性逐渐增强 ;增加引发剂和共聚单体MMA的浓度 ,粒子的水化半径逐渐减小 ,粒径分散系数增大 .     

Synthesis and Crystal Structure of N-cyclopropyl-9 -（3,4-dicholophenyl）- 1,2,3,4,5,6,7,8,9,10-decahydroacridine -1,8-dione under Microwave Irradiation

1 INTRODUCTION aryl or methyl group to the nitrogen atom of these compounds leads to enhanced activities of fluo- A lot of natural and synthetic compounds con- rescence[7, . Since the pyridine scaffold is included 8] taining acridine skeletons display interesting biolo- in decahydroacridine-1,8-dione, a question is whether gical and physical activities[1]. Acridinedione, for the same modification on the nitrogen atom of de- example, has been identified as antimalarial and cahydroacridine-1…     

Thermal and microwave-assisted N-formylation using solid-supported reagents

A rapid and easy route to formamides by microwave assisted N-formylation of primary and secondary amines is described. Using an insoluble polymer or an inorganic solid-supported reagent as a formylating agent, microwave irradiation furnished the corresponding formamides in high yields, with reduced reaction time and solvent volume over the conventional approach.     

Comparison of the Temperature Effect on the π∗←n and π∗←π Electronic Transition Bands of NO<Subscript>3</Subscript><Superscript>−</Superscript>(aq)

The effect of temperature on the π∗←π transition band in the UV absorption spectrum of NO₃⁻(aq) centered at ≈200 nm was studied in the temperature range 10–70 ^∘C. The observed temperature independence of this band was in contrast to the significant influence of temperature on the nitrate π∗←n transition reported recently by us. However, taking into account the electronic states involved in both the transitions, it was concluded that this finding was in accordance with our previous assumption that interconversion between spectrally distinct (with respect to π∗←n band) nitrate species included the rupture/formation of hydrogen bond(s) in the hydration shell of the nitrate ion.