黄酮类药物与氯金酸的作用及其分析应用

将4种黄酮类药物染料木素、木犀草素、大豆素及柚皮素与氯金酸在不同酸度条件下反应形成金纳米颗粒. 研究发现, 生成的金纳米颗粒的等离子体共振吸收信号与4种黄酮类药物的浓度呈线性关系, 从而建立了这4种典型黄酮类药物的测定方法. 分析了黄酮类药物的分子结构并利用Materials-studio 4.0软件计算了各原子的电子云密度分布. 结果表明, 4种黄酮类药物与氯金酸作用的适宜酸度与黄酮类化合物结构中的酚羟基数和碱性氧的电子云密度分布有关.     

铅离子选择性电极检测终点间接电位测定大蒜中大蒜辣素含量

取新鲜蒜瓣试样若干，捣成糊状。称取约50．00g，加浓硝酸20mL处理使其中所含亚砜基氧化成20mL，加水，过滤并定客。分取此滤液一份（约十分之一），置于滴定杯中，用氢氧化钠溶液调酸度至pH5～6，加入一倍体积的乙醇，以铅离子选择电极指示终点，用铅标准滴定溶液进行电位滴定。终点电位预先用二次微商法求得。方法所测得结果的RSD为0．44％，且与重量法测定结果相比无显著差异。     

在线酸坝富集-毛细管区带电泳法测定槐角中的染料木素

建立了分离测定槐角提取液中染料木素的在线酸坝富集-毛细管区带电泳方法,考察了酸的种类、酸的及浓度、进样/进酸时间比例等因素对堆积效率的影响.实验以20mmol/L硼砂(pH 10.5)作为缓冲溶液,200mmol/L柠檬酸溶液(pH 1.7)作为酸坝,进样、进酸时间分别为180s和45s,在分离电压15kV,检测波长2...     

虫草素的合成

以腺苷为原料经原酸酯环化和乙酰溴水解原酸酯、自由基还原脱溴及水解乙酰基等3步反应合成了虫草素——3'-脱氧腺苷,总收率29.8%,纯度95%,其结构经1H NMR和MS确证。     

马兜铃酸极谱研究

用单扫示波极谱法研究马兜的电化学行为。在０．１ｍｏｌ／ＬＮａＯＨ底液中，马兜铃酸在－０．８９Ｖ产生一良好的二阶导数 极谱峰，线性范围为０．０３－３２ｍｇ／Ｌ检出限为０．０１ｍｇ／Ｌ。     

11-巯基十一酸-(8-生物素酰胺基-3,6-二氧辛基)酰胺的合成

以溴十一酸、苄硫醇、生物素和长醚链二胺为原料,通过活化酯法,设计并合成了一种新型长链含巯基的生物素衍生物--11-巯基十一酸-(8-生物素酰胺基-3,6-二氧辛基)酰胺,其结构经<'1>H NMR和IR表征.     

中药和葡萄糖酸锌治疗儿童缺锌性厌食100例

对100例经微量元素检查均有缺锌和厌食表现的儿童，用中药和葡萄糖酸锌治疗，并与单纯用葡萄糖酸锌治疗50例作为对照，结果中药和葡萄糖酸锌治疗效果好，厌食较快好转。     

ICP-AES法测定钢中酸溶铝和酸不溶铝及全铝

应用ICP－AES法测定了钢中酸溶铝和酸不溶铝，并对测定条件及相关参数进行了试验和优化，并于基体的干扰及方法的准确度和精密度也作了研究并标准物质作了验证。用此法所测得结果与标准物质的证书值间无显著差异，将酸不溶铝和酸溶铝的测得值相加即得总铝的量。     

冠醚方酸碲碳菁染料的合成研究

合成了不对称冠醚方酸碲碳菁染料和对称冠醚方酸碲碳菁染料，并探讨了对称冠醚方酸碲碳菁的合成方法及反应条件，提出了其可能的反应机理。     

掺杂质子酸的类型对聚苯胺结构和电导率的影响

采用化学氧化聚合法以苯胺为单体，过硫酸铵为氧化剂，在不同质子酸的水溶液中合成聚苯胺，考察质子酸对聚苯胺电性能影响，并通过傅立叶红外吸收光谱（FTIR）和紫外可见光吸收光谱（UV－vis)研究聚苯胺掺杂前后结构的变化。结果表明，龙质子酸掺杂后聚 胺具有导电性是因为其分子链上电荷离城形成了共轭结构，具有不同质子酸中生成的聚苯胺氧化程度不同；分子链共轭程度与掺杂酸对阴离子大小有关，掺杂质子酸对阴离子越大，聚苯胺分子链共轭程度越大，电导率也就越高。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

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.