Investigation of Isomerization of 2—Seleno—1,3,2—diazaphospholidine Derivatives

For the first time the isomerization of 1,3,2-diazaphospholidine-2-sclenide dervatives in refluxing benzene in the presence of trace water was observed. The structures of isomerized products were determined by IR, ^1H NMR,^31P NMR, elemental analysis and X-ray crystallography. The mechanism of isomerization was also proposed.     

(2E,4E)-3-苯基-2-[2-(N-乙氧羰基甲基氨基)-苯硫基]-2,4-己二烯酸乙酯——一个新的分子内重排反应产物

２，３－二氢－２－甲基－４－苯基－１，５－苯并硫氮杂卓与重氮乙酸乙酯反应，得到非预期的分子内重排的开环产物。通过元素分析、ＩＲ，１ＨＮＭＲ，ＭＳ及Ｘ－晶体衍射分析确定了它的结构，并根据产物的结构，对这一新反应的反应机理进行了探讨和研究。     

微波辐射下三组分“一锅法”合成5-芳基-1,5,6,7,8,9-六氢化-2H-吡唑[5,4-b]并喹啉-6-酮

在微波辐射下以芳醛、1,3-环己二酮或达米酮和氨基吡唑为原料, 用乙二醇作能量转移剂, 三组分“一锅法”快速合成了一系列吡唑[5,4-b]并喹啉类化合物. 该方法速度快(30～90 s), 产率高(88%～98%), 环境友好. 产物结构通过红外光谱、核磁共振谱和元素分析证实, 化合物4e的单晶经X射线衍射分析, 进一步确证了产物结构.     

Synthesis and Characterization of Novel Organosoluble Methyl Substituted Poly(aryl Ether Ketone)s Containing Sulfone Linkage

Several new methyl substituted poly(aryl ether ketone)s containing sulfone linkage with inherent viscosities of 0.62–0.84 dL/g have been prepared from 4,4′‐bis(2‐methylphenoxy)diphenylsulfone and 4,4′‐bis(3‐methylphenoxy)diphenylsulfone with terephthaloyl chloride and isophthaloyl chloride by electrophilic Friedel‐Crafts acylation in the presence of DMF with anhydrous AlCl₃ as a catalyst in 1,2‐dichloroethane, respectively. These polymers having weight‐average molecular weight in the range of 71,000–49,000 are all amorphous and show high glass transition temperatures ranging from 167 °C to 191 °C, excellent thermal stability at temperatures over 400 °C in air or nitrogen, high char yields of 51–58% in nitrogen and good solubility in CHCl₃ and polar solvents such as DMF, DMSO and NMP at room temperature.     

几种卟啉在化学还原沉积银膜上的表面增强拉曼光谱特征

应用 Ｊｏｂｉｎ－Ｙｖｏｎ Ｕ—１０００型拉曼光谱仪和ＬＡＢＲＡＭＩ型拉曼光谱系统研究了 ３种卟啉ＴＯＨＰＰ、ＴａｍＰＰ和ＴＳＰＰ在化学还原沉积法制备的银膜上的ＲＳ和ＳＥＲＳ光谱特征。结果表明：化学还原法制备的银膜可以作为这几种卟啉的拉曼增强活性载体。这３种卟啉在获谱的过程中都形成二聚态化合物和发生银离子搀和作用，较长的放置和测谱时间有利于银离子的搀和。     

Ni-P/SiO_2催化剂晶化过程及其加氢活性研究

采用化学还原法制备了负载型Ni－P／SiO2非晶态合金催化剂．应用ICP、BET、氢氧滴定法、XRD、SEM、XPS研究了上述催化剂在高温晶化过程中的表面结构、表面形貌和表面电子态的变化。测定了Ni－P／SiO2非晶态合金晶化前后对其液相苯甲醛加氢反应催化活性和选择性,并讨论了非晶态合金催化剂晶化过程中结构变化对催化性能的影响．     

A NEW ONE-STEP REDUCTIVE N-ALKYLATION OF AMINO ACIDS AND THEIR ESTERS

The reductive alkylation of amine with carbonyl compounds usingsodium hydrogen telluride has been investigated in recent years.Application of this method to the synthesis of N-alkyl derivativesof biologically important amino acids and their esters is described.     

水杨酸与烟草铜锌超氧化物歧化酶的相互作用

利用邻苯三酚自氧化法监测了磷酸盐缓冲体系中水杨酸（SA）对超氧化物歧化酶（SOD）活力的影响。通过荧光光谱法研究了水杨酸与超氧化物歧化酶的相互作用机制，求得两者结合的形成常数和配位数，使用Forster非辐射能量转移技术求出了两者的结合位置距色氨酸残基间的距离为2.60nm。     

A New β-Carboline Alkaloid and a New Derivate of Isoferulic Acid from Anemone altaica

A new β-carboline alkaloid, 4-（9H-β-carbolin-1-yl）-4-oxobutyric acid and a new derivate of isoferulic acid, （E）-3-（3-hydroxy-4-methoxyphenyl）acrylic acid carboxymethyl ester, were isolated from the roots of Anemone altaica. Their structures were determined on the basis of spectral data.     

Influence of neutral cyclodextrin concentration on plate numbers in capillary electrophoresis

A quantitative theory of plate number N in capillary electrophoresis was developed for buffers containing neutral cyclodextrins (CDs) capable of forming inclusion complexes. In the theory, N was modeled by longitudinal diffusion, injection extent, width of the detection window, and the detector time constant. The apparent mobility was modeled as a weighted sum of the mobilities of the free-solution analyte and the inclusion complex. The apparent diffusion coefficient was modeled as a similarly weighted sum. Both the apparent mobility and diffusion coefficient were corrected by functions that compensated for increases of buffer temperature caused by Joule heat. The experimental N's and apparent mobilities of neutral thiourea and of the anions, dansyl D- and L-leucine, dansyl D- and L-aspartic acid, benzoate, and 4-nitrophenolate, were determined in buffers containing from 0 to 15 mM beta-CD. The binding constants, and mobilities and diffusion coefficients of the free-solution analyte and inclusion complex, were calculated as regression coefficients by fitting theory to these determinations. The regression coefficients were shown to have physicochemical meaning, as assessed by literature values, independent measurements, and theoretical predictions. The assessment showed the Nernst-Einstein equation does not relate mobilities and diffusion coefficients at the electrolyte concentration used. The interdependence of mobilities, diffusion coefficients, binding constants, and other dispersion sources was interpreted to evaluate the factors affecting the variation of N with CD concentration. From the interpretation, an approximate equation for N in low-concentration CD buffers was derived. The equation depends on free-solution and inclusion-complex mobilities and diffusion coefficients, the binding constant, the potential difference over the effective capillary length, and the number of plates in a CD-free buffer.