芳胺转化为酰芳胺的方法

按照形成酰胺键所用原料分类,可将芳胺酰基化分为羧酸衍生物法、羧酸法和其他方法。羧酸衍生物法主要有酰氯法和酸酐法;羧酸法主要有偶联法、TAPC研磨法、P(OMe)3/I2催化法、纳米MgO催化法;其他方法主要是乙腈法、N,N-二甲基乙酰胺法、Au/HAP催化下的羟基合成法。     

气相色谱中多种死时间测定方法的比较

由烷烃同系物的保留时间计算死时间的方法有多种,常用的并得到认可的有Grobler-Balizs法(G-B法)、Guaradino法(G法)、Peterson-Hirsch法(P．H法)和Ambms法(A法)等。文献[5]已证明A法和G-B法是同一的。本文是文献[5]的继续,将证明A法、P-H法和G法也是同一的。     

废弃油脂生产生物柴油的研究进展

简单介绍了生物柴油的生产原料,综述了用废弃油脂生产生物柴油的现状和方法。废弃油脂生产生物柴油的方法主要有物理法和化学法,物理法主要有掺和法和微乳法,化学法主要有热裂解法和酯交换法。目前生产中采用化学法的酯交换法、以酸碱两步催化法的工艺为主,而生物酶法和超临界法是研究热点。     

遗忘因子法与其它计算方法在分光光度法中的应用研究

本文考查了常规最小二乘法、Ｐ－矩阵法、主成份回归法、偏最小二乘法、线性规划法、卡尔曼滤波以及遗忘因子法对安痛定注射液模拟样品的分析结果。从所得结果来看，遗忘因子法有一定的优点。     

杜马斯燃烧法与连续流动法测定再造烟叶中总氮量的比较

为提高检测再造烟叶中总氮含量的检测效率,对杜马斯燃烧法(简称D法)和连续流动法(简称L法)进行了对比研究,并初步探索了转换D法结果来代替L法结果的方法。结果表明:杜马斯燃烧法结果普遍高于连续流动法结果,两种方法均具有良好的精密度和准确度。在提高检测效率、降低人员劳动强度和环境污染方面,杜马斯燃烧法优势明显。杜马斯燃烧法结果应用比值系数K(K=DN/LN)进行换算即可代替连续流动法结果。     

化妆品车间空气消毒方法效果比较

评价几种消毒方法对化妆品车间空气的消毒效果。分别使用紫外线照射消毒法、甲醛蒸熏消毒法、戊二醛消毒液气溶胶雾化消毒法、臭氧气体发生器消毒法4种方法进行消毒,然后用平皿沉降法进行采样评价分析,试验结果表明,戊二醛消毒法和臭氧消毒法可以代替紫外线消毒法和甲醛消毒法进行化妆品车间空气常规消毒。     

AES法和AAS法测定食品、药物中微量元素的进展

综述了80年代以来原子发射光谱（AES）法和原子吸收光谱（AAS）法在食品和药物中微量元素分析的应用进展，内容包括，样品的预处理和进样技术，ICP-AES法和其他AES法。FAAS法，GFAAS法，HG-AAS法和冷蒸气AAS法等方面的应用及发展状况。     

电子气体中水分检测方法

介绍冷镜式露点法、阻容法、电解法、转化法、卡尔·费休库仑法、光学法、石英晶体振荡法的检测原理、特点和应用。冷镜式露点法适用于大多数无特殊性质的气体中水分的检测；阻容法响应快，适合在线检测；电解法操作简便、精度高、成本低；转化法针对性强，样品量小；卡尔·费休库仑法检测限低、精度高；光学法检测限低，且适合腐蚀性、有毒气体中的水分检测；石英晶体振荡法具有量程宽的优势，应用广泛。     

稀土发光材料的合成方法

简要介绍了合成稀土发光材料的6种方法,包括水热合成法、溶胶-凝胶法、微波辐射法、燃烧合成法以及共沉淀法。参考文献31篇。     

氧化石墨烯分离膜机械性能调控

氧化石墨烯(Graphene oxide, GO)片层组装制备的分离膜,具有可调控的纳米通道和独特的分离性能,是一种很有前景的分离材料,但较差的机械性能制约了其实际应用。将活性分子、阳离子等粒子引入到GO膜的片层间,利用其与GO形成的稳定键合可提高GO膜的机械性能。本文综述了国内外在GO膜机械性能调控方面的研究进展。依据引入的粒子与GO成键的类型可分为共价键法和非共价键法,其中共价键法又分为大分子共价键法和小分子共价键法,非共价键法分为氢键法、π-π键法和离子键法。无论共价键法还是非共价键法都能显著提升GO膜的机械性能,其中共价键法对GO复合膜的增强效果优于非共价键法,大分子共价键法优于小分子共价键法。最后,阐述了现有方法存在的问题,并对未来的发展前景做出了展望。     

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.