N-bound primary nitramines based on 1,5-diaminotetrazole

1,5-Diaminotetrazole can be nitrated under very mild conditions by using nitronium tetrafluoroborate to result in 5-amino-1-nitriminotetrazole (1) in good yields. The same reaction can be performed with 1-amino-5-amino-4-methyltetrazole to yield 5-amino-4-methyl-1-nitriminotetrazole (2). Both compounds have been isolated and completely characterized by using vibrational spectroscopy, mass spectrometry, and differential scanning calorimetry. Additionally, X-ray diffraction measurements of the neutral compounds could be obtained; they indicated the structure of both compounds to be zwitterionic. Compounds 1 and 2 exhibit extremely high sensitivities to impact and friction and high positive heats of formation of 496 (1) and 453 kJ mol(-1) (2), respectively. Additionally, high-nitrogen-containing salts of 1 have been synthesized by metathesis reactions of silver 5-amino-1-nitriminotetrazolate with the corresponding halides so as to investigate the changes in sensitivity and thermal stability. All ionic compounds have been synthesized in good yields and characterized by means of vibrational and multinuclear NMR spectroscopy as well as X-ray diffraction measurements. Thermal stabilities have been evaluated by differential scanning calorimetry, whereas sensitivity measurements have been performed according to standardized Bundesanstalt für Materialforschung und -prüfung (BAM) tests. Theoretical calculations have been performed to investigate the heats of formation as well as the performance characteristics of the compounds.     

4(6)-{2-[4-(2,3,4-三甲氧基苄基)哌嗪-1-基]-2-氧代乙氧基}芳甲酰胍类化合物的合成及其Na~+/H~+交换器1抑制活性

NHE1(Na+/H+交换器1)抑制剂对于心肌缺血再灌注损伤具有较好的保护作用.以苯(或吡啶)甲酰胍为母核,利用拼合原理,在苯(或吡啶)甲酰胍母环上引入4-(2,3,4-三甲氧基苄基)哌嗪-1-甲基,设计并合成了8个未见文献报道的目标化合物.其结构经MS,IR,1H NMR和元素分析确证.体外血小板肿胀模型(PSA)试验结果表明,大部分目标化合物显示出较好的NHE1抑制活性.     

8-5’新木脂素类化合物的合成方法研究

对羟基桂皮酸甲酯和阿魏酸甲酯分别在氧化银催化下发生自由基仿生氧化偶联反应, 合成得苯并二氢呋喃环结构化合物1, 1经甲基化反应得2. 1a和1和2分别在无水碳酸钾、10%氢氧化钠水溶液等不同的碱性条件下进行反应, 获得了11个苯并二氢呋喃环开环产物, 即8-5’新木脂素类化合物3a～9b, 实现了由苯并二氢呋喃新木脂素向8-5’新木脂素的转变, 也为合成芪类化合物提供了一种新方法. C-8位上的吸电子基团如酯基的影响使苯并二氢呋喃环易在碱性条件下开环形成8-5’新木脂素类化合物．所合成化合物的结构由MS, IR, 1H NMR和13C NMR进行了表征.     

NO2‐Fe (II)Pc‐catalyzed synthesis of 2‐ferrocenyl‐5‐aryl‐1,3,4‐oxadiazoles and study of antifungal activity

Six novel derivatives of 2‐ferrocenyl‐5‐aryl‐1,3,4‐oxadiazoles have been synthesized through catalytic oxidation of benzoylhydrazone with nitrophthalocyanine iron (II) as catalyst and tert‐butyl hydroperoxide as oxidant. All of the compounds have been characterized by high‐resolution mass spectrometry, ¹H, ¹³C NMR, and infrared spectroscopy. Moreover, the antifungal activities of all new compounds have been evaluated and the results showed that the compounds exhibited excellent antifungal activities. In addition, the molecular structure of compound 1c could also be determined by X‐ray single‐crystal diffraction.     

N-取代苄基-4-羟基-4-取代哌啶衍生物的合成及初步抗白血病活性

为了寻找对白血病细胞系增殖有较高抑制活性的先导化合物,本文以取代苄胺为原料,经Michael加成,Dieckmann缩合,水解脱羧和与Grignard试剂反应合成了12个均未见文献报道的目标化合物6a─6l,结构均经过1H NMR、IR、MS及元素分析确证。并采用MTT法对目标化合物进行了对白血病K562细胞系增殖影响的初步测试,结果表明大部分具有较好的抑制细胞系增殖的活性,有潜在的抗白血病活性。     

New Azidotetrazoles: Structurally Interesting and Extremely Sensitive

The treatment of triaminoguanidinium chloride with two equivalents of sodium nitrite under acidic conditions, followed by the cyclization with stoichiometric amounts of either sodium hydroxide solution or solid sodium carbonate yielded 1‐amino‐5‐azidotetrazole ( 1 ), 5‐azido‐1‐diazidocarbamoyltetrazole ( 2 ), and 1‐(aminoazidocarbamoyl)‐5‐azidotetrazole ( 3 ). The three novel compounds could be isolated by short‐column liquid chromatography by using chloroform in reasonable yields. The mechanism of the formation as well as the decomposition pathway of the materials was investigated and a full characterization of all three compounds is presented. Compounds 1 , 2 , 3 have been characterized by means of Raman and IR as well as multinuclear NMR spectroscopy, mass spectrometry, and X‐ray diffraction studies. Thermal stabilities have been evaluated by differential scanning calorimetry. Theoretical calculations have been performed to ensure the assignment of the vibrational modes obtained from Raman and IR measurements. The sensitivity values obtained from our measurements reflect the behavior of the compounds, which show an extremely high sensitivity toward mechanical as well as thermal stimuli.     

用低温DTA测定熔点及作相图

DTA法是一种动态测量技术,可在程序变温情况下对给定物质或体系提供一个连续的、以温度或时间为函数的物性变化信息。通常测低温的熔点和相变用卡计,一般用样品20—30g。低温DTA只需1—3mg样品,而且一个样品可扫描出几个熔点。     

芳酰基吡咯里嗪衍生物的设计与合成

COX和5-LOX双重抑制剂通过同时阻断炎症介质前列腺素和白三烯的形成, 产生协同的抗炎作用, 可以提高疗效, 同时避免COX抑制剂引发的副作用. 以芳基吡咯里嗪为先导物, 设计合成了2类15个5或6位芳酰基取代的7-芳基-2,3-二氢-1H-吡咯里嗪衍生物进行抗炎活性研究; 也可以其为模板进行结构修饰与优化, 设计合成更好的COX/5-LOX双重抑制剂. 同时分析了同分异构体III和IV的波谱学性质, 并确证了化合物的结构.     

Separation of some amino acids by supercritical fluid chromatography after a pre-derivatization step with classical reagents

Summary The separation of polar compounds by supercritical fluid chromatography is a difficult problem to solve. In this work, we have used a pre-derivatization method to obtain apolar or less polar compounds. Amino acids have been chosen as model polar compounds of biological interest, and 9-fluorenylmethyl chloroformate (FMOC) and (+)-1-(9-fluorenyl)ethyl chloroformate (FLEC) have been used as derivatizating reagents.With this procedure, the amino acids studied have been separated in less than 40 minutes with a good efficiency. Furthermore, with FLEC reagent, the enantiomeric separation was rapid in comparison with liquid chromatography techniques and the selectivities obtained were in the same order of magnitude.     

Synthesis and properties of aminomethoxy derivatives of 1-(butylsulfanyl)pentane

New aminomethoxy derivatives of 1-(butylsulfanyl)pentane have been synthesized. The structure of the synthesized compounds was studied by elemental analysis, IR and ¹Н NMR spectroscopy, and mass spectrometry. Some specimens of the synthesized compounds were tested as antimicrobial additives to lubricant oil, and as aseptic compounds against bacteria and fungi.     

苯并噻唑螺萘并噁嗪类化合物的微波合成与性质

以苯并噻唑衍生物、1-亚硝基-2-萘酚为原料,三乙胺为催化剂,无水乙醇为溶剂,采用微波辐射法合成了苯并噻唑螺萘并噁嗪光致变色化合物.通过元素分析,IR,MS,1H NMR对结构进行了表征,并用紫外分光仪研究了溶剂效应和荧光分光光度计研究了荧光效应,结果表明该类化合物具有较好的荧光性能,其开环体的λmax与溶剂的极性常数呈较好的线形相关性.     

Virtual Screening of Natural Compounds as Potential PI3K-AKT1 Signaling Pathway Inhibitors and Experimental Validation

A computational screening for natural compounds suitable to bind the AKT protein has been performed after the generation of a pharmacophore model based on the experimental structure of AKT1 complexed with IQO, a well-known inhibitor. The compounds resulted as being most suitable from the screening have been further investigated by molecular docking, ADMET (Absorption, Distribution, Metabolism, Excretion, and Toxicity) analysis and toxicity profiles. Two compounds selected at the end of the computational analysis, i.e., ZINC2429155 (also named STL1) and ZINC1447881 (also named AC1), have been tested in an experimental assay, together with IQO as a positive control and quercetin as a negative control. Only STL1 clearly inhibited AKT activation negatively modulating the PI₃K/AKT pathway.     

Nitrogen bridgehead compounds,part 68. Studies on quinolizine derivatives. Part 2. Synthesis of 1,3-disubstituted-4H-quinolizine derivatives

Quinolizine compounds 1 and 2 or their monocyclic tautomers 3 and 4 have been synthesized using 2-pyri-dineacetic acid derivatives 6a, b, A, B and ethoxymethylenemalonic acid derivatives 7a, b, c in base catalyzed or thermic reaction. In the 6-unsubstituted series, both the 4-oxo and 4-imino derivatives could have been obtained, in the 6-substituted series, however the 4-oxo ones only, whereas instead of the 4-imino derivatives, their monocyclic tautomers 3, 4 have been isolated. In the 6-unsubstituted series, the primarily formed 4-imino compounds have been rearranged into 4-oxo ones under stronger conditions. The structure of the isolated compounds have been proved by ultraviolet, infrared and ¹H nmr spectra, that of 3B=C by X-ray analysis as well.     

Weak molecular associations investigated by 1H-NMR spectroscopy on a neat organosiloxane-solvent mixture

The rational design of new sensitive materials for chemical sensors relies on the knowledge of molecular interactions between the chemical species in question with compounds that may potentially be present in the gas phase. In this context, the intermolecular interactions between a family of functionalized polysiloxanes and a series of organic compounds have been investigated. This work addresses the problem of determining the association constant or energy by studying neat liquid mixtures without solvents. An original approach has been proposed to obtain such information from the excess function of the difference in chemical shifts between both interacting species. Data obtained as a function of the composition of the mixtures have been fitted according to two models: either by considering the formation of a 1:1 complex governed by an equilibrium constant or by the existence of a local composition following the Wilson model. Both methods have been tested on model compounds and the results have been compared with solubility enthalpies calculated using Hansen coefficients.     

Recovery of all species from photolytic degradation of tributyltin compounds TBTX (X = Cl,OSn Bu3)

Malformations in shellfish have been reported by many authors. They attributed the cause of the deformity to the presence in water of organotin compounds used in the formulation of antifouling paints, for example bis(tributyltin) oxide (TBTO) and tributyltin chloride (TBTC). The behaviour of these compounds has been examined under abiotic laboratory conditions. The influence of many parameters such as sunlight, pH, oxygen, salinity have been examined. The degradation compounds obtained have been identified: (1) In the gas phase two major products, butene-1 and buetene-2, are observed with consumption of oxygen; (2) In the liquid phase, three main products are obtained, butanol-1, butanol-2 and butanone 2. The identified products represent a small part of the total concentration, suggesting a competing process such as formation of butyltin polymers; (3) In fresh water an amorphous solid phase is observed while in seawater a white cristalline precipitate appears.     

新荧光试剂4-氨基安替比林芳香席夫碱的合成

新荧光试剂4-氨基安替比林芳香席夫碱的合成     

SYNTHESIS AND ANTIMICROBIAL SCREENING OF SOME NEW 4-IMINO-3,5,7-TRISUBSTITUTED PYRIDO[2,3-d]PYRIMIDINES AND THEIR RIBOFURANOSIDES AS POTENTIAL CHEMOTHERAPEUTIC AGENTS

Some new nucleosides, viz. 4-imino-3,5,7-trisubstituted-1-(2′,3′,5′-tri-O-kbenzyl–β-D-ribofuranosyl)pyrido[2,3-d]pyrimidin/e–2(1H)-ones/ thiones(VII/VIII), have been synthesized by condensation of trimethylsilyl derivatives of 4-imino-3,5,7-trisubstituted pyrido[2,3-d]pyrimidin/e-2(1H)-ones/thiones (III/IV) with β-D-ribofuranosyl1-acetate-2,3,5-tribenzoate. Compounds III/IV have been synthesized by refluxing 2-amino-3-cyano-4,6-disubstituted pyridine (II) with substituted an arylisocyanate or an isothiocyanate respectively. The structure of all the synthesized compounds have been established by IR and ¹H NMR studies. These compounds have been screened for antimicrobial activities in order evaluate. The possibility of the derivatives to be used as potential chemotherapeutic agents.     

Banana-shaped mesogens: effect of 2-methylresorcinol as the central unit on the mesomorphic properties of five-ring esters

Three homologous series of banana-shaped five-ring esters and one series of seven-ring esters derived from 2-methylresorcinol have been synthesized. This has been carried out to understand the effect of chemical structure on the mesomorphic properties of such compounds. It is shown that the 2-methyl substituent in the central phenyl ring destabilizes the mesophases when they are compared with those of the analogous unsubstituted compounds. Replacement of a phenyl ring by a biphenyl moiety (seven-ring esters) in the two arms of the bent-core molecule enhances the thermal range of the mesophases as well as the clearing temperatures. The mesophases have been characterized using techniques such as polarizing optical microscopy, differential scanning calorimetry, and X-ray diffraction, and by electro-optical investigations. In the 32 compounds investigated, two mesophases, B 1 and B 2 , have been identified.     

吲哚-6-酰腙类化合物的微波合成及其抗菌活性研究

把酰腙类结构引入吲哚环中, 合成一类新型的吲哚-6-酰腙化合物, 以期为新药筛选提供先导化合物. 在微波辐射条件下, 以较高的产率得到14个未见报道的新化合物, 其结构均经1H NMR, IR, MS及元素分析确证, 并测试了化合物的抑菌活性.     

Synthesis and characterization of novel quinoline selenium compounds: X-ray structure of 6-methoxy-3H-[1,2]diselenolo[3,4-b]quinoline

A series of novel and synthetically important quinoline selenium compounds have been successfully synthesized using an efficient and simple strategy. The method employed leads to the synthesis of both cyclic as well as open chain quinoline selenium compounds. The prepared selenium compounds have been characterized with the help of various spectroscopic techniques viz., NMR (¹H, ¹³C), FT-IR, mass spectrometry. The structure of 6-methoxy-3H-[1,2]diselenolo[3,4-b]quinoline has been determined by X-ray crystallography.