稠杂环化合物研究

稠杂环化合物研究ＸＩ．３－（３′－吡啶基）－６－芳基－均三唑并［３，４－６］－１，３，４－噻二唑的合成张自义，王作祥，郑国钰（兰州大学化学系，７３００００）众所周知，均三唑及１，３，４－噻二唑化合物均具有广泛生物活性，如抗菌￣［１，２］，抗病毒，抗肿...     

基于2-卤苯甲酰胺合成苯并杂环化合物的研究进展

苯并稠杂环化合物具有广泛且重要的药理及生物活性,在药物合成与研发领域有着重要的应用价值,因而其合成方法倍受关注.由于存在多个官能团和反应位点,以2-卤代苯甲酰胺为重要合成子合成喹唑啉酮、异喹啉酮、异吲哚酮和苯并异噻唑酮等苯并杂环化合物取得了巨大进展.鉴于此,根据产物结构的不同,概述近10年来以2-卤苯甲酰胺为起始原料合成苯并杂环化合物的研究进展,并对相关的反应机理进行了阐述.     

喹唑啉稠合螺杂环化合物的合成及晶体结构

许多螺杂环化合物及喹唑啉化合物具有抗癌、消炎、抗真菌、抗细菌、抗结核、抗肿瘤以及除草等生物活性,将噻唑酮和喹唑啉稠合环结构与螺杂环结构合为一体,合成新的喹唑啉稠合螺杂环化合物,以期得到具有更高生物活性的化合物,是当前化学家研究的课题之一,1,3-偶极环加成反应是合成五元杂环的常用方法,采用环外双键结构的化合物为亲偶极体,     

3-氯-4-氰基-5-取代苯氧基异噻唑的合成及生物活性

有些醚化合物如早期出现的商品化品种草枯醚、间草醚等二苯醚类除草剂 ,其结构相对简单、在土壤中易于降解且易于合成 ,因而引起了人们的广泛[1 - 3] 兴趣。最近的研究表明很可能从异噻唑杂环中找到生物活性独特的新型化合物[4] 。为此 ,我们设计合成了含异噻唑杂环的醚类化合物3ａ～ 3ｋ ,合成路线见下图 .所有产物经1 ＨＮＭＲ、ＩＲ和元素分析证实 ,并对大部分化合物的除草活性和杀菌活性进行了测定。1　实验部分所有溶剂为分析纯 ,用前经纯化处理。试剂为化学纯或分析纯。硅胶为青岛海洋化工厂产品。元素分析用ＹａｎａｃｏＣＨＮＣＯＲ…     

硫脲化合物的合成及其生物活性

硫脲化合物的合成及其生物活性董燕红，司宗兴（北京农业大学应用化学系北京１０００９４）关键词噻二陛－甲酰基，硫脲，胺类，合成，生物活性酰基硫脲在抗真菌、抗结核、抗病毒、除草以及调节植物生长方面具有广泛应用［１，２］。１，２，３－噻二唑杂环作为有效前体正...     

新型吡唑腙类化合物的合成

吡唑肼作为合成含氮杂环的中间体为人们广泛关注, 为了寻找可能具有生物活性的杂环化合物, 设计并合成了两类新型含有吡唑基的腙类化合物, 其结构经¹H NMR, IR, MS和元素分析确证. 初步的除草与杀菌活性测定表明它们具有一定的活性.     

香草醛—N—酰腙类化合物的合成与表征

Ｓｃｈｉｆｆ碱类化合物和酰腙类化合物大多具有除草,杀菌等生物活性,已有一些报道［１,２］,对该类化合物的深入研究是当今农药界热点之一,表明此类化合物具有广阔的开发前景。据文献报道［１］,香草醛与芳胺反应生成的Ｓｃｈｉｆｆ碱类化合物具有优异的促进植物生根性。为寻求新的具有生物活性的物质,我们采用香草醛与酰肼反应,合成了３种未见报道的酰腙类化合物。其结构经ＩＲ,１ＨＮＭＲ和元素分析证实。合成反应如下：３—ＣＨ３Ｏ—４—ＨＯＣ６Ｈ３ＣＨＯ＋Ｈ２ＮＮＨＣＯ—Ｒ３—ＣＨ３Ｏ—４—ＨＯＣ６Ｈ３ＣＨＮＮＨＣＯ…     

新型含噻唑环的吡唑肟醚类衍生物的合成及其生物活性

为了寻找活性较好的杂环农药,将噻唑基团引入到吡唑分子结构中,设计合成了一系列新型含噻唑环的吡唑肟醚衍生物.通过1H NMR、13C NMR和元素分析测试对标题化合物的结构进行了表征.对合成的目标化合物进行了初步的生物活性测试,部分化合物显示出一定的的杀菌、杀虫或植物生长调节活性.     

酰胺缩醛法合成N,N,N′-三取代甲脒的研究

酰胺缩醛法合成Ｎ，Ｎ，Ｎ′┐三取代甲脒的研究张娟刘毅锋（西北大学应用化学研究所西安７１００６９）脒类化合物用作杀螨、杀虫剂，除草剂，消炎剂等［１，２］，也是合成氮杂环化合物的中间体［３］。有关脒的合成及应用研究的进展，我们已进行了较为详细的评述［４］...     

含氮杂环羧酸基二（三）苄基锡配合物的合成

烃基氯化锡及其衍生物具有广泛的生物活性,如杀虫、杀菌、抗癌等。近年来已有较多报道［１］,但关于杂环羧酸基烃基锡配合物的合成研究报道则很少,而含氮杂环羧酸基苄基锡配合物的合成研究尚未见文献介绍。为寻找具有更高生物活性的有机锡配合物,本文以二（三）苄基氯...     

碳苷研究 V: 用Grignard试剂合成取代苯酚中酚羟基的保护及脱保护

本文报道了一些取代苯酚的合成, 并探讨了用Grignard试剂合成取代苯酚中酚羟基的保护及脱保护的问题. 利用苄基和甲基作为酚羟基的保护基, 对文献报道的切断醚键脱保护方法进行了评价. 找到了两种新体系能在更温和条件下切断醚键的方法, 指出了它们的适用条件. 实验结果符合硬软酸碱理论.     

FT-IR, FT-Raman spectra, density functional computations of the vibrational spectra and molecular geometry of biomolecule 5-aminouracil

FT-IR and FT-Raman spectra of the biomolecule 5-aminouracil were recorded in the regions 400–4000 cm⁻¹ and 10–3500 cm⁻¹, respectively. The observed vibrational wavenumbers were analyzed and assigned to different normal modes of vibration of the molecule. Density functional calculations were performed to support wavenumber assignments of the observed bands. A comparison with the molecule of uracil was made, and specific scale factors were employed in the predicted wavenumbers of 5-aminouracil. With the purpose of study the important molecule 5-aminouracil, its equilibrium geometry and harmonic wavenumbers were calculated for the first time by the B3LYP DFT method. The vibrational wavenumbers were compared with IR and Raman experimental data. Also good reproduction of the experimental wavenumbers is obtained and the % error is very small. All the tautomeric forms of 5-aminouracil were determined and optimized. The dimer forms were also simulated. The energy, atomic charges and dipole moments were discussed and several general conclusions were underlined.     

南瓜籽烘烤前后化学成分的分析

对烘烤前后南瓜籽中的化学成分进行分析并对比。采用同时蒸馏萃取装置萃取南瓜籽中的挥发性成分,采取超临界CO2萃取技术萃取南瓜籽油脂,并将其分为酸、碱、中性三个部分,用气相色谱-质谱联用方法分析其中化学成分并进行对比。结果表明,南瓜籽挥发性成分中含有多种醛类和酯类化合物,烘烤后产生了大量的烷基吡嗪,其在碱性部分中的相对含量比烘烤前提高14倍多,不饱和醛类化合物含量也有明显提高。南瓜籽油脂中的主要化学成分是油酸、亚油酸及其酯类。还含有生物活性功能成分如植物甾醇、角鲨烯和维生素E等。烘烤后除角鲨烯含量有所降低,维生素E、植物甾醇、亚麻酸等均有提高。     

Preparation and properties of polyurethane networks based on α,ω-difunctional poly(hexafluoropropylene oxide)

Poly(hexafluoropropylene oxide), poly(HFPO), networks were prepared from functional polymers by end linking via urethane groups. The prepolymers were characterized by NMR spectroscopy and GPC. The networks were characterized by determination of the number of network chains from the shear modulus, and were snown to contain both trifunctional crosslinks and difunctional links. The properties of the networks were investigated by a range of techniques. Compared with fully-fluorinated networks formed via triazine cross-links, investigated previously, the urethane-linked networks were more readily prepared but were poorer elastomers, were less thermally stable, and were less resistant to swelling by common polar solvents. © 1995 John Wiley & Sons, Inc.     

Synthesis,Luminescence and Intramolecular Energy Transfer of Binary and Ternary Rare Earth Complexes with Aromatic Carboxylic Acids and 1, 10-Phenanthroline

A series of binary and ternary rare earth complexes with para-substitued benzoic acids and 1,10-phenanthroline were synthesized. The phosphorescence spectra were measured and the lowest triplet state energies of ligands were determined, the phosphorescence lifetimes were obtained and intramolecular energy transfer mechanism between ligands was studied. The luminescence properties were also measured and were in agreement with the prediction. The energy match and intramolecular energy transfer process in these binary and ternary complexes were discussed in detail.     

ADSORPTION OF PHENOL AND NITROPHENOLS ON A HYPERCROSSLINKED POLYMERIC ADSORBENT

The adsorption of phenol and nitrophenols on hypercrosslinked polymeric adsorbent wasstudied as a function of the solution concentration and temperature. Adsorption isotherms of phenoland nitrophenols on hypercrosslinked resin were determined. These isotherms were modeledaccording to the Freundlich adsorption isotherm. The isotherms for phenol and nitrophenols onhypercrosslinked resin were assigned as L curves. Thermodynamic parameters were calculated for allphenol and nitrophenols. The kinetics experiment results showed that the adsorption rates were of thefirst-order kinetics. The rate constants at 303K were calculated.     

Mg/Al型水滑石吸附硼的实验研究

采用共沉淀法制备了几种不同摩尔比的镁铝水滑石(LDHs),并对其进行了XRD、FT-IR表征.将其应用于吸附溶液中的硼,比较了它们对硼的吸附容量,最终选择了具有较高吸附容量的Mg4Al-LDH作为硼吸附荆.对Mg4Al-LDH吸附硼的实验条件进行了系统研究,得到了较高吸附容量下的实验条件.试验结果表明该等温吸附过程可用Langmuir吸附等温模型准确描述.     

Effect of Alkyl Chain Length of N-Alkyl-N′-(2-benzylphenyl)ureas on Gelation

Urea derivatives that were substituted with a 2-benzylphenyl group and an alkyl group functioned as low molecular weight gelators for various organic solvents and ionic liquids. Urea derivatives with long alkyl chains were effective for the gelation of polar solvents. However, they were not suitable for the gelation of non-polar solvents, whereas urea derivatives with short alkyl chains were effective. Ionic liquids were similar to polar solvents in that urea derivatives with long alkyl chains were the most effective gelators. The physical properties of the formed supramolecular gels were analyzed by dynamic viscoelasticity measurements using a rheometer.     

Preparation of Titania/PDMS Hybrid Films and the Conversion to Porous Materials

Transparent films of titania/poly(dimethylsiloxane) (PDMS) hybrids were prepared by the solvent evaporation from the precursor solution prepared by the co-hydrolysis and co-condensation of titanium tetraisopropoxide and a methoxy-functionalized PDMS. The hybrid films were flexible and had high homogeneity of the composition. The organic groups of PDMS were decomposed at 400°C in air to form porous films. Though the heated films were rather brittle compared to the as-synthesized films, they were still transparent and homogeneous. The BET surface areas of the films after the heat treatment at 400°C were over 300 m²/g, while the as-synthesized hybrid films were non porous. According to the BDDT classification, the nitrogen adsorption/desorption isotherms of the calcined films were Type I, showing that the films were microporous. The titania domains were still amorphous after the heat treatment at 400°C and transformed to anatase after the heat treatment at 1,000°C.     

Polyimide-Silica Hybrids: Spectroscopy,Morphology and Mechanical Properties

Polyimide/silica hybrids were prepared by a sol-gel process and were evaluated in terms of curing behaviour, morphology and mechanical properties. The spectroscopic examination showed that the presence of the inorganic phase accelerates the imidization of the polyamic acid. Two types of morphology for the silica phase were obtained by tailoring the composition of the precursor solution mixture. The mechanical properties were found to be strongly dependent on the system morphology. The largest increase in rigidity and strength properties were achieved when the two phases were co-continuous.