微波辐射下苯并(口恶)唑基吡啶的合成

含有苯并唑基的杂环化合物由于其特殊的生理活性而广泛用作医药、农药[1];因为具有较高的荧光量子产率,还可作为荧光增白剂、闪烁剂[2]等。现有合成方法反应时间长[3,4],而且需高温下进行。微波辐射下的有机合成具有反应时间短、产率高的特点[5]。本文在微波辐射条件下,利用邻氨基酚和吡啶羧酸的缩合反应,合成了2种苯并唑基取代吡啶。其优化反应条件为:多聚磷酸为催化剂,微波输出功率为500W,辐射时间4分钟。相比于常规反应,该条件下的反应速率是常规加热法反应速率的60倍且产率有所提高。合成路线如下:ppA=Polyphosphoricacid1　…     

微波固相法合成钠快离子导体Na5YSi4O12

应用微波方法合固相反应难于制备的Ｎａ５ＹＳｉ４Ｏ１２纯相，讨论了微波合成条件对产物的影响，与溶胶－凝胶法相比，微波法反应速率快，选择性强，合成的样品具有特异的聚集态，缺陷和微结构，从而导致离子导电活化能下降。     

N-丙基-N-[2-(2,4,6-三氯苯氧基)乙基]-1H-咪唑-1-甲酰胺的合成

以2，4，6-三氯苯酚和1，2-二氯乙烷为初始原料，在相转移催化剂十六烷基三甲基溴化胺和弱碱性助剂三乙胺存在下合成了N-丙基-N-[2-(2，4，6-三氯苯氧基)乙基]-1H-咪唑-1-甲酰胺，其结构经元素分析,IR，^1H NMR分析证实。并对该合成路线的反应机理进行了讨论。     

吡咯基金属络合物的制备及其在有机合成中的应用

本文综述了近年来吡咯基金属络合物的研究进展, 详细讨论了σ~N-、σ~C-、π-型吡咯基金属络合物的制备方法, 以及各类吡咯基金属络合物在有机合成中的应用。     

Stopped-flow injection analysis. The influence of diffusion on dispersion of normal and reverse flow injection

A relationship is derived to enable the comparison of the dispersion heights of normal and reverse flow injection analysis (FIA). A single channel flow system is employed in the absence of a chemical reaction. The stopped-flow injection method is used to probe the influence of molecular diffusion on the overall dispersion of normal and reverse FIA, which appeared to demonstrate fundamentally different diffusion behaviors. Small discrepancies are observed between the dispersion heights, which are enhanced by the stopped-flow period, especially when unmatched matrix ionic compositions of the indicator and counter solutions were involved. For these conditions, the diffusion flux rate is enhanced considerably, displaying a peak, in addition to the transient, for both methods. The influence of diffusion on the dispersion characteristics of normal and reverse FIA is discussed theoretically. Diffusion in the proposed model is postulated to oppose dispersion by convection. The latter initiates concentration gradients in the injection zone and propagates it with flow time over the dispersion zone profile. The diffusion flux then reacts in order to confine the indicator dispersion for normal FIA and to enhance it for reverse FIA. This model is consistent with the experimental results and accounts for most of the phenomena encountered. Probably owing to the influence of secondary flow phenomena, the use of coiled tubes has suppressed the effects of diffusion on the overall dispersion behavior.Part of the experimental work was performed at IMI Institute for Research and Development, Haifa, Israel.     

有机溶剂中(R)-醇腈酶催化不对称合成(R)-苯乙醇腈

 研究了来源于杏仁的（R）－醇腈酶在有机溶剂异丙醚中催化苯甲醛与HCN不对称合成（R）－苯乙醇腈，初步探讨了来源于不同杏仁的（R）－醇腈酶的筛选、最适酶量的确定以及底物HCN与苯甲醛的配比、底物浓度、酶的微环境pH和反应温度对不对称合成反应的影响．结果发现，来源于苦杏仁的（R）－醇腈酶优于来源于甜杏仁的（R）－醇腈酶．优化的反应条件为：最适酶量150g／L，HCN与苯甲醛的配比2．5，苯甲醛浓度300mmol／L，酶的微环境pH5．4，反应温度0～5℃．在该优化反应条件下，反应平衡转化率和产物的光学纯度均高达99％以上．     

血小板阻聚药物中间体N-环己基-5-氯丁基-1H-四氮唑的合成

以δ-戊内酯和环己胺为原料合成了抗血小板聚集药物西洛他唑的重要中间体N-环己基-5-氯丁基-1H-四氮唑，选择了合适的相转移催化剂及安全的叠氮试剂并获得较高的收率。     

Potential of X-Ray Diffractometry in Structure Identification of Holmium Polysulfides

A series of experiments have been carried out to synthesize holmium polysulfides at temperatures from 600 to 840°C and sulfur vapor pressures of (2.1, 6.5, 16.7)á10⁵ Pa. Polysulfide crystals sized up to 2 mm and micron-sized powders were investigated thereafter by powder diffractometry. Powder diffraction patterns were calculated based on our previous X-ray structural data. Characteristic reflections have been revealed for the individual monoclinic and tetragonal phases, and X-ray phase analysis (XRPA) has been performed for all batches of the synthesis. The monoclinic phase is shown to prevail irrespective of the synthetic conditions. The tetragonal phase was found in amounts of up to 10 wt.%.     

Characterization of chemiluminescence from singlet oxygen under laminar flow conditions in a micro-channel and its quenching with beverages

Singlet oxygen was generated by reaction of sodium hypochlorite and hydrogen peroxide in a micro-channel. The two reagent solutions were delivered into the micro-channel by a syringe pump, providing a laminar flow liquid-liquid interface. The chemiluminescence from the singlet oxygen was emitted in the collapse of the interface due to molecular diffusion under laminar flow conditions. The chemiluminescence intensity was observed continuously and stably for each combination of reagents fed into the micro-channel; while, in the normal batch-type reactor the chemiluminescence peaks from singlet oxygen were observed within ca. 5 s. The features of the chemiluminescence emitted under laminar flow conditions were examined by changing the concentrations of sodium hypochlorite and hydrogen peroxide; the concentrations of 2.5 mM sodium hypochlorite and 7.5 mM hydrogen peroxide provided highest chemiluminescence intensities without bubble formation. Also, the effects of beverages, such as green tea, coffee, white wine, red wine, and sake (rice wine), on the chemiluminescence intensity as well as the concentrations of sodium hypochlorite and hydrogen peroxide were examined. The chemiluminescence intensities observed with addition of the beverages to the reagents decreased in the following orders; green tea > coffee > red wine > rice wine > white wine (being added to sodium hypochlorite); coffee > white wine > green tea > red wine > rice wine (being added to hydrogen peroxide). It was found that coffee decreased the chemiluminescence intensity (ca. 33% chemiluminescence decrease) without altering the concentrations of sodium hypochlorite or hydrogen peroxide. The cause of the decrease in chemiluminescence with coffee is discussed.     

Synthesis of diterpene glycosides

Summary Mono-, di-, and linear triglycosides of a diterpene alcohol, derived from abietic acid and glucose have been synthesized employing peracetylbromo--D-glucose (4) and maltose derivatives5 and8 as glycosyl donors. The triglycoside14 exhibits slight haemolytic activity.

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Synthese von Diterpenglycosiden

Zusammenfassung Es wird die Synthese von Mono-, Di-, und linearen Triglycosiden aus einem von Abietinsäure abgeleiteten Diterpenalkohol beschrieben. Als Glycosyldonoren wurden neben Peracetobrom--D-glucose (4) die Maltosederivate5 und8 verwendet. Das Triglycosid14 zeigt schwache hämolytische Aktivität.