用理学3064X荧光仪分析碳

在理学３０６４Ｘ荧光仪上采用十八烷基马来酸（ＯＨＭ）晶体作为色散单元，通过改造电路，调整晶体倾角，获得对碳分析的良好线性，在流气正比计数器（ＦＰＣ）窗膜分别为５μｍ和０．６μｍ条件下，碳元素的峰背比分别达到３８．９１和５４．０４。作者分析了白口铸铁和碳化硅中的碳，结果表明在理学３０６４Ｘ荧光仪上定量分析碳是可行了，具有快速、简便、准确、多元素同时分析的特点，可用于日常分析     

（C5H7S2）3[Bi2Cl9）]的合成和晶体结构

标题化合物由ＢｉＣｌ３和乙酰丙酮在ＨＣｌ（气）／Ｃ２Ｈ５ＯＨ溶剂中通入Ｈ２Ｓ气体反应而得。晶体属四方晶系，Ｍｔ＝１１３０．７６，空间群Ｐ４１２１２。晶胞参数ａ＝ｂ＝８．８６７（２），ｃ＝４１．５１１（４）Ａ；Ｖ＝３２６４（１）Ａ＾３，Ｚ＝４，Ｄｃ＝２．３０ｇｃｍ＾－３，μ（ＭｏＫａ）＝１１８．６０７ｃｍ＾－１，Ｆ（０００）＝２１０４．晶结构由重原子法求得。最终偏离因子Ｒ＝０．０７２。晶体由分立的（     

甘氨酸间硝基苯甲酸晶体比热容的测定—差示扫描时热法（DSC）

论述用ＤＳＣ及比热软件测量甘氨酸间硝基苯甲酸（Ｇ．ｍＮＢＡ）晶体比热容的方法。以蓝宝石为标样，测量Ｇ．ｍＮＢＡ晶体的比热容，其相对平均偏差在０．０８％～０．４７％之间。     

雪松二醇—（R）—1—苯基甲基硼酸酯（phCHClBO2C15H24）的不对称合成和 …

利用雪松二醇苯基硼酸酯进行不对称合成反应，制得标题化合物并测定结构，其晶体属正交晶系，空间群为Ｐ２１２１２１。结果学参数为：ａ＝５７２８（３），ｂ＝８．５４３（３），ｃ＝４１．２６７（７）Ａ，Ｖ＝２０１９．７Ａ＾３，Ｚ＝４，Ｄｃ＝１．２３ｇ＝ｃｍ＾３，μ（ＣｕＫα）＝１７．７ｃｍ＾－１，Ｒ＝０．００７２，Ｒω＝０．００７７。     

^—P421m相掺钕钼酸钆晶体的结构

标题的晶体是采用提拉法得到的,单晶Ｘ射线结构分析表明：化合物分子式（Ｎｄ０．０２３Ｇｄ０．９７７）２（ＭｏＯ４）３晶体属于四方晶系,空间群为＾－Ｐ４２ １ｍ,ａ＝ｂ＝７．３５５６（１０）,ｃ＝１０．６８５（２）＾°Ａ,Ｚ＝２,Ｄｃ＝４．５６３ｇ／ｃｎｍ＾３。Ｍｒ＝１５８５．６４,Ｆ（０００）＝７００．００,μ（ＭｏＫａ）＝１４．５２７ｃｍ＾－１、Ｒ＝０．０４６３,ｗＲ＝０．０９５３,衍射点数为６４     

（Y（NTO）2NO3（H2O）5）.2H2O的制备,晶体结构和热分解机理的…

合在了（Ｙ（ＮＴＯ）２ＮＯ３（Ｈ２Ｏ）５）．２Ｈ２Ｏ（ＮＴＯ为３－硝基－１，２，４－三唑－５－酮）并测定了晶体结构，晶体属单斜晶系，空间群Ｃｍ，晶胞参数：ａ＝０．６７７３（２）ｎｍ，ｂ＝２．０８６６（２）ｎｍ，ｃ＝０．６５５１（１）ｎｍ；β＝１０２．９８（２）°Ｖ＝０．９０２１（１）ｎｍ＾３，Ｚ＝２，Ｄｃ＝１．９７０ｇ．ｃｍ＾－３，μ＝３３．４９ｃｍ＾－１，Ｆ（０００）＝５４０，Ｒ＝０．０３２，中     

小晶粒A型分子筛的合成及其晶貌

分子筛晶粒的大小对分子筛的催化、吸附及离子交换性能均具有很大的影响．以常规方法合成的Ａ型分子筛，其晶粒大小一般分布在１～１０μｍ，平均粒径大于２μｍ，并且样品中含有３％～１２％超过４５μｍ的大晶粒［１］．在合成过程中，凝胶混合物的配比、成胶和晶化条件...     

丁基罗丹明B—钼酸盐光度法连续测定铈和钪

在聚乙烯醇（ＰＶＡ）存在下，丁基罗丹明Ｂ（ＢＲＢ）分别与铈钼、钪钼杂多酸络阴离子形成离子缔合物，其最大吸收均位于５７０ｎｍ，表面摩尔吸光度分别为εＣｅ＝３．９６×１０＾６Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，εＳｃ＝４．７１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，服从比耳定律范围分别为０－２４μｇ／Ｌ Ｃｅ和０－６０μｇ／ＬＳｃ，测定极限为Ｃｅ１．０μｇ／Ｌ（ｎ＝１２）和Ｓｃ１．９μｇ／Ｌ（ｎ＝１０），对     

三硒化二饵Er2Se3的合成与结构

采用高温固相反应和化学气相传输法合成三硒化二饵，晶体属于四方晶系Ｍｒ＝５７１．４０，空间群为Ｐ４／ｎｍｍ，ａ＝３．９８４（１），ｃ＝８．２２８（３），Ａ，Ｖ＝１３０．５９（７）Ａ＾３，Ｚ＝１，Ｄｃ＝７．２７ｇ／ｃｍ＾３，Ｆ（０００）＝２３８，μ（ＭｏＫａ）＝５２８．８６ｃｍ＾－１，对于１８７个Ｉ≥３σ（１）的独立衍射点，最后偏离因子Ｒ＝０．０６６，Ｒｗ＝０．０７８，化合物Ｅｒ２Ｓｅ３的晶体结构是由     

3,3—二甲基—9—（5,5—二甲基—3—羟基—2—环己烯—1—酮—2—基）—1—氧代—2 …

标题化合物Ｃ２３Ｈ２６Ｏ４是水杨醛与５，６－二甲基－１，３－环己二酮在Ｎ，Ｎ－二甲基甲酰胺中反应而得。结果通过单晶Ｘ－射线衍射法确定，其晶体属于单斜晶系，空间群Ｐ２１／ｃ，ａ＝７．０５６，ｂ＝２０．２６３，ｃ＝１３．６６５Ａ，β＝９３．３２，Ｖ＝１９５０．７Ａ＾３，Ｍｒ＝３６６．４６，Ｄｃ＝１．２４８ｇ／ｃｍ＾３，Ｚ＝４，μ（ＭＯＫα）＝０．８４ｃｍ＾－１，Ｆ（０００）＝７８４。晶体结构用直接法解     

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.