铵盐与酰氯的酰胺化合成伯酰胺（英文）

报道了一种以简单、易得的氯化铵为胺源,合成伯酰胺的酰胺化方法.以N-甲基吡咯烷酮(NMP)为溶剂和缚酸剂,在加热的条件下各种脂肪酰氯和芳香酰氯都能与氯化铵快速地反应,以良好到优秀的收率得到相应的伯酰胺,该反应为伯酰胺的合成提供了一种快速、实用的方法.     

高选择性N-单甲基化芳香胺的合成

本文报道了一种高效专一性合成N-单甲基芳胺的方法。芳胺先与醋酐反应生成乙酰胺,再与碘甲烷在氢化钠作用下反应生成相应的N-甲基乙酰芳胺。在乙二醇中用酸水解高产率得到相应的N-单甲基芳胺。并将该方法用于药物中间体的合成。     

烷酰氧基芳磺酸盐的合成研究

研究了以羧酸酐和羟基芳磺酸盐为主要原料,丙酮为溶剂、无水碳酸钠为缚酸剂的烷酰氧基芳磺酸盐的清洁合成工艺,制备了4-壬酰氧基苯磺酸钠(NOBS)、壬酰氧基尼文酸钠、4-甲基丙烯酰氧基苯磺酸钠、甲基丙烯酰氧基尼文酸钠等4个化合物.考察了合成反应的影响因素.结果表明,以对羟基苯磺酸钠和壬酸酐为原料合成4-壬酰氧基苯磺酸钠(N...     

N-(芳亚甲基)芳胺Schiff碱汞化反应区域选择性研究

本文用量子化学的MNDO方法对N-(苯亚甲基)苯胺、N-(苯亚甲基)-2-甲苯胺与N-(4-硝基苯亚甲基)-2-甲氧基苯胺Schiff碱汞化反应区域选择性进行了研究,结果表明,在其稳定构象下,芳胺环上的电荷密度大于苯基亚甲基环, 故汞化反应发生在芳胺环上；分子中亚胺氮原子的电荷密度最大, 在汞化反应过程中, 亚胺氮原子首先与醋酸汞配位,然后再进行邻位亲电进攻,生成邻位汞化产物；而在N-(苯亚甲基)-2-甲苯胺分子中, 邻位甲基阻碍了亚胺氮原子与汞原子的配位作用,故无邻位汞化产物生成。计算结果与实验结果一致, 并进一步支持了已经提出的反应机理。     

N—甲基—N—芳基—2—（4‘—硝基苯硫基）乙酰胺类化合物的合成

先由芳胺合成N-甲基芳胺,再由氯乙酰氯酰化后与对硝基硫酚在相转移催化条件下反应,生成2-(4＇-硝基苯硫基)乙酰芳胺.该法具有操作简便,产率高的优点.     

N-方酰麻黄碱配体的合成及催化前手性芳酮的不对称还原反应

方酸与醇反应成方酸二酯,后者与天然麻黄碱反应得到N-方酰麻黄碱或N-方酰双麻黄碱。单N-方酰麻黄碱与脂肪胺及硫氢化钠等反应合成了C-3位含氮和含硫的系列配体。首次将这些方酰麻黄碱配体经原位制备手性恶唑硼烷催化前手性芳酮及二酮的不对称还原反应,得到化学产率和e.e.值分别为85%-98%和52.5%-87.4%的手性仲醇。新化合物的结构已IR,^1H NMR,MS和元素分析所证实,化合物4b的晶体结构用X射线射确认。     

N-甲基-N-芳基-2-(4''''-硝基苯硫基)乙酰胺类化合物的合成

先由芳胺合成 N-甲基芳胺 ,再由氯乙酰氯酰化后与对硝基硫酚在相转移催化条件下反应 ,生成 2 -(4 -硝基苯硫基 )乙酰芳胺。该法具有操作简便 ,产率高的优点。     

均苯三甲酰胺-胺的合成及表征

以均苯三甲酰氯(TMC)和1,3-二氨基-2-丙醇(DAP)为原料,通过酯化、酰胺化和酯胺解反应,合成了树枝状大分子化合物均苯三甲酰胺-胺(TMAAM),并优化了合成工艺.考察了甲醇用量、缚酸剂种类及用量和原料DAP用量等对反应收率的影响,分析了酯胺解反应机理.用红外光谱(IR)、核磁(NMR)和高分辨质谱(HRMS)分析了TMAAM的化学结构.该合成方法反应条件温和,操作简单,后处理方便,并具有较高的反应经济性,产品收率最高可达57%.     

三芳胺合成的研究进展

三芳胺化合物的合成方法主要有3种:(1)非金属催化的胺化反应;(2)铜催化的Ullnann反应,包括使用过量铜粉为催化剂的传统的Ullmann反应、使用相转移催化剂的Ullmann反应以及使用配体的post-Ullmann反应;(3)钯催化的Buchwald-Hartwig反应.该类反应活性的关键是配体的选择,根据配体结构的不同可分为双膦螯合型配体、单膦配体和非膦配体.对该类化合物的这几种合成方法的研究进展进行了总结.     

N-甲基-N-芳基-2-(4＇-硝基苯硫基)乙酰胺类化合物的合成

先由芳胺合成N-甲基芳胺,再由氯乙酰氯酰化后与对硝基硫酚在相转移催化条件下反应,生成2-(4＇-硝基苯硫基)乙酰芳胺.该法具有操作简便,产率高的优点.     

飞行时间二次离子质谱(TOF-SIMS)结合化学衍生法分析杂环新化合物的结构

飞行时间二次离子质谱(TOF-SIMS)分析了难挥发的杂环新化合物咪唑啉硫氰酸盐及其三种衍生物, 确认出很强的氢离化及银离化准分子离子峰, 通过对各种衍生物谱图的对照分析, 确认出较强的含有结构特征的碎片离子峰, 并对该化合物在离子轰击下的裂解规律作了分析, 支持了对该新化合物结构的鉴定。     

3-芳氧基-6-取代哒嗪的合成及其除草活性

合成了系列3-芳氧基-6-取代哒嗪类化合物.化合物结构经¹HNMR、元素分析、IR和MS确证.生物活性测试结果表明,该类化合物具有很好的除草活性,讨论了其结构与除草活性的关系.     

A Plasma Surface Treatment of Polyester Textile Fabrics Used for Reinforcement of Car Tires

Polyester tire cord surfaces have been modified by plasma at low temperature and atmospheric pressure. The surface treatment has been executed by various nonequilibrium discharges, namely by barrier discharge, atmospheric pressure glow discharge and gliding arc. The polymeric multicord sewing threads treated by this procedure have been used in the same form as in industry, i.e., with the protecting oil films on their surface. The surface properties have been investigated by electron spin resonance spectroscopy and by measuring their contact angle with various liquids; partially the zeta potential measurements have been used, too. Further tests have been done at an industrial testing impregnation line using the common technology and conditions, on both plasma treated and untreated fibers. Finally, the standard H-tests and peel-tests have been used to characterize the fiber adhesion to usual testing rubbers.     

High-performance quantitative thin-layer chromatography of flavonoid glycosides and biflavonoids ofCupressus sempervirens in relation to cypress canker

Summary The flavonoid glycosides and the biflavonoids of cypress leaves have been separted by means of high-performance thin-layer chromatography with quantitation by densitometry. Some flavonoid glycosides and biflavonoids have been identified, other than from their chromatographic characteristics, by means of UV spectra recorded directly on the layer. Different clones, resistant and susceptible to cypress canker, have been analyzed; some differences between these two classes of trees have been found in their biflavonoid content.     

Synthesis of monodisperse spherical nanocrystals

Much progress has been made over the past ten years on the synthesis of monodisperse spherical nanocrystals. Mechanistic studies have shown that monodisperse nanocrystals are produced when the burst of nucleation that enables separation of the nucleation and growth processes is combined with the subsequent diffusion-controlled growth process through which the crystal size is determined. Several chemical methods have been used to synthesize uniform nanocrystals of metals, metal oxides, and metal chalcogenides. Monodisperse nanocrystals of CdSe, Co, and other materials have been generated in surfactant solution by nucleation induced at high temperature, and subsequent aging and size selection. Monodisperse nanocrystals of many metals and metal oxides, including magnetic ferrites, have been synthesized directly by thermal decomposition of metal-surfactant complexes prepared from the metal precursors and surfactants. Nonhydrolytic sol-gel reactions have been used to synthesize various transition-metal-oxide nanocrystals. Monodisperse gold nanocrystals have been obtained from polydisperse samples by digestive-ripening processes. Uniform-sized nanocrystals of gold, silver, platinum, and palladium have been synthesized by polyol processes in which metal salts are reduced by alcohols in the presence of appropriate surfactants.     

Polymer modification to achieve novel properties

Polymers have been modified, by subjecting them to reactions in solution, in the melt and in the solid state. Novel polymers with improved and optimized properties have also been created by copolymerization, chain transfer or by the design of chain termination. Even by manipulating the initiation step in polymerizations, functional and reactive groups have been introduced at the head of the polymer chain. Polymer properties have been modified by influencing physical properties of polymers by orienting, annealing and blending.     

相转变温度范围窄的聚(N-异丙基丙烯酰胺)温敏性微凝胶

采用间歇式、半间歇式和连续式无皂乳液聚合(SFEP)法合成温敏性聚(N-异丙基丙烯酰胺)(PNIPAM)微凝胶。连续式或半间歇式SFEP法合成的PNIPAM微凝胶相转变温度范围明显地比间歇式SFEP法合成的窄,其中又以连续式SFEP法的效果最明显。相同交联剂用量的情况下,连续式SFEP法合成的PNIPAM微凝胶的粒径和溶胀比最大,而间歇式SFEP法合成的最小。通过研究微凝胶合成过程中溶胀比随反应时间的变化关系,证明了连续式或半间歇式SFEP法合成的PNIPAM微凝胶具有比较均匀的内部交联结构。     

硫酸锌与L-亮氨酸配合物行为的研究

锌是生命元素,缺锌引起的各种疾病已引起全世界的共同注意.L-α-氨基酸是人体蛋白质的基本结构单元.α-氨基酸锌作为添加剂在药物、食品和化妆品中有广阔的应用前景[1～3].L-α-亮氨酸(简写为Leu)是人体必需但在人体内又不能合成的氨基酸之一,必须从食物中得到.文献中尚未见亮氨酸锌的报导.本文用半微量相平衡方法[4]研究了ZnSO4-Leu-H2O体系在25℃的相化学行为,发现该体系中未形成新化合物.改进文献方法合成了未见文献报导的Zn(Leu)SO4·12H2O和Zn(Leu)2固态配合物,并研究了它们的物理化学性质.1实验部分1.1试剂与仪器　　Zn…     

The Structure of the Elusive Simplest Dipeptide Gly-Gly

Among the hundreds of peptide compounds for which conformations have been determined by using different spectroscopic techniques, the structure of the simplest dipeptide glycylglycine (Gly-Gly) is conspicuously absent. Herein, for the first time, solid samples of Gly-Gly have been vaporized by laser ablation and three different structures have been revealed in a supersonic expansion by Fourier transform microwave spectroscopy. The intramolecular hydrogen bonding interactions that stabilize the observed forms have been established based on the ¹⁴N nuclear quadrupole hyperfine structure. We have illustrated how conformer interconversion distorts the equilibrium conformational distribution, giving rise to missing conformers in the conformational landscape.     

Curing of an epoxy resin modified with poly(methylmethacrylate) monitored by simultaneous dielectric/near infrared spectroscopies

Simultaneous dielectric and near infrared measurements have been performed in “real-time” to follow polymerisation reactions on blends of a diglycidyl ether of bisphenol-A epoxy resin with 4,4^′-diaminodiphenylmethane hardener and different amounts of poly(methylmethacrylate) as modifier. The effect of the modifier amount on the polymerisation reactions has been studied, as well as that of the curing temperature. Epoxy and amine conversions have been followed by near infrared spectroscopy (NIR), while changes in molecular mobility in the reaction mixture have been analysed by dielectric relaxation spectroscopy (DRS). Evolutions of ionic conductivity and α-relaxation have been analysed and vitrification times have been obtained. The relaxational behaviour has been analysed through curing in the frequency domain, being the change of the main relaxation indicative of the cure reaction advancement. DRS data are also presented as complex impedance Z(ω). Vitrification times, obtained by dielectrometry have been compared with those obtained by rheological measurements and gelation times obtained by NIR have been compared with those obtained by solvent extraction.