AlN粉末合成新方法研究

氮化铝（ＡｌＮ）是一种性能优异的工程材料。目前，ＡｌＮ粉末的合成方法虽有多种，但真正能用于工业生产的只有铝粉直接氮化法和碳热还原法。其它方法如化学气相沉积法、裂解法和等离子化学法因生产成本非常昂贵，只能用于实验研究。即使是目前工业上常用的那两种方法，...     

计算机辅助分子设计的三维结构搜寻方法

三维结构搜寻是一种新型的计算机辅助分子设计方法。本文对表征三维结构的信息来源、三维结构搜寻基本方法及其在药物分子设计中的应用作了较系统的综述，它不仅可用于先导化合物的优化，更重要的是有用于新型先导化合物的发展。此外，它也可用于新型农用化学品、材料、催化剂和聚合物的开发。     

高效液相色谱梯度洗脱同时测定化妆品中防腐剂、抗氧化剂和杀菌剂

建立了一种灵敏、快速的高效液相色谱梯度洗脱同时测定化妆品中防腐剂、抗氧化剂和杀菌剂的方法。采用C8柱，以甲醇和水为流动相梯度洗脱。在检测波长273nm用二极管阵列检测器，17min内可将4种防腐剂、2种抗氧化剂和2种杀菌剂分离测定。方法快速准确，用于实际样品的测定。     

四极质谱计与微机的联用

本文介绍一种将四极质谱计与微机联用简易方法，可实现对气体样品连续，快速和自动分析，并提出一种新的质谱数据解析方法，可用于多组分气体样品常规定量分析。     

用于色氨酸分离测量的仪器

本发明涉及一种用于色氨酸分离测量的仪器，包括最高转速大于5000r／min的离心机、吸放装置、加样装置、以及控制装置，所述离心机包括孔数M的离心转盘，所述M个孔可分为N组，每组包括3个孔分别用于承载第一离心管、第二离心管和第三离心管，所述控制装置用于执行以下步骤：（a）控制所述离心机旋转以分离第一离心管中血样的血清；（b）控制所述吸放装置吸取所述第一离心管中的血清加入到第二离心管和第三离心管；     

一种新的预报策略

本文提出一种新的预报策略，将校准和预报的测量数据结合在一起进行主成分分解，找到校准和预报的共同的正交投影空间。这种新策略用于确定主成分数的交叉验证时只需一次主成分分解，因此速度很快；用于定量预报时，模型稳定性好，预报准确度令人满意。     

一种电化学分析仪

本实用新型提出一种电化学分析仪，包括用于将电化学信号转变为电信号的电极控制装置；用于设置电极控制装置工作状态的数字输入输出电路，与电极控制装置连接；用于采集电极控制装置的数据并将其转换为数字信号的数据采集转换器，与电极控制装置连接；用于接收数据采集转换器采集的数据并进行数据处理的控制装置，与数据采集转换器连接；用于接收控制装置的数据并将其转换为电极控制装置的控制信号的信号发生器，分别与控制装置和电极控制装置连接；无线传输装置，与控制装置连接；用于连接外接存储装置、显示器、键盘、鼠标和以太网的接口，与控制装置连接；电源装置，与控制装置连接。本实用新型集成度高、体积小、便于随身携带。     

一种新型毛细管电泳—电感耦合等离子体光谱法接口装置

毛细管电泳是一种高效、简便的分离方法，已被用于生物、环境及临床等试样的分离及分析[1]．检测技术在毛细管电泳中占有重要的地位，目前，在柱紫外可见及荧光检测是两种广为接受的检测方法，但其检测灵敏度仅为10－5～10－6mol／L[2]．电感耦合等离子体光谱（ICP－AES／MS）是一种灵敏的元素选择性的分析方法，已被广泛地用于各种试样中元素分析．近年来，该方法作为色谱及毛细管电泳的检测器，被用于元素的形态分析[3]．在毛细管电泳（CE）与ICP光谱连用技术中，挑战性的工作是设计一种能把CE与ICP相连的接口．目前已有几种接口…     

丙烯基苯化合物改性双马来酰亚胺树脂：Ⅰ.BPPDPS的合成,表…

合成了一种双丙烯基苯化合物－双（丙烯基苯氧基）二苯砜用于 改性双马来酰亚胺。根据Ｗｉｌｌｉａｍｓｏｎ法合成了双（丙烯基苯氧基）二苯砜，并用于元素分析、红外光谱、紫外光谱、核磁共振、质谱等方法进行了结构表征。测定了预聚物的溶解范围，获得了溶解性较好的混合溶剂，用于复合材料成型加工。     

绿色简易法制备纯二氧化氮气体

设计了一种在密闭容器中制备纯二氧化氮气体的绿色简易方法。该方法实现了气体制备、收集、尾气处理的一体化，不仅可用于课堂演示实验，也为深入研究二氧化氮溶于水的定量实验奠定物质基础。另外，此方法也可用于无氧环境下其他物质的制备。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.