基于双苯并咪唑及二羧酸配体配合物的合成、结构及抗菌活性

利用双苯并咪唑基配体4,4′-二(苯并咪唑-1-甲基)联苯(bbmb)与V形二羧酸配体4,4′-二羧苯基醚(H2dcpe)合成了配合物{[Ni(bbmb)(dcpe)(H_2O)]·2H_2O}_n(1)和{[Mn_2(bbmb)(dcpe)_2(H_2O)]·1.5H_2O}_n(2)。通过红外、元素分析、X射线单晶衍射、热重分析等检测手段对配合物结构进行了表征。配合物1是具有sql拓扑构型的二维层状化合物。配合物2呈现出含有四核锰构型的二维层状结构。体外抗菌实验证明2个配合物都表现出良好的抗菌活性。     

连翘果实中的三个新化合物

利用大孔吸附树脂柱色谱、Sephdex LH-20凝胶柱色谱以及半制备高效液相色谱等技术,从连翘果实的乙醇提取物中分离得到三个新的化合物,包括两个苯乙醇苷类衍生物forsyside A(1),forsyside B(2)以及一个倍半萜forsysacid A(3).通过UV,IR,HRESIMS,一维NMR和二维NMR...     

双酰基脲新化合物的合成与杀虫活性

报道了含双酰基脲新化合物的合成，经元素分析、IR、^1HNMR确定了新化合物的结构，部分化合物具有良好杀虫活性。     

在醋酸中用锌粉还原蒽醌制备4种新化合物

在醋酸中用锌粉还原蒽醌制备4种新化合物;蒽醌;还原;醋酸;锌     

儿茶素-稀土配合物的合成、表征及抗菌活性

以稀土(Re³⁺)和儿茶素(C)为原料,由液相合成法制备了3种(La³⁺-C、Gd³⁺-C、Er³⁺-C)配合物,结合傅里叶变换红外光谱、紫外光谱、X射线光电子能谱及配位数测定对配合物结构进行表征,确定了配合物的配位数为8。并采用牛津杯法、最小抑菌浓度(MIC)及最小杀菌浓度(MBC)等三种方法测定了Re³⁺-C对大肠杆菌、金黄色葡萄球菌、绿脓杆菌、沙门氏菌4种食源性细菌的抗菌性能。结果表明,这3种稀土配合物对各试验菌株均表现不同程度的抑制能力,相较Re³⁺和C而言,Re³⁺-C配合物的抑菌性能均有显著的提高。Re³⁺-C的抑菌活性顺序为：Gd³⁺-C > La³⁺-C > Er³⁺-C,其中Gd³⁺-C对4种细菌的MIC值分别为：1.550、0.097、0.780、1.550 μmol·mL⁻¹,MBC值分别为3.100、0.194、1.550、1.550 μmol·mL⁻¹,Gd³⁺-C对金黄色葡萄球菌表现出最佳的抑菌和杀菌能力。     

棘孢曲霉中分离的2个新化合物

从土壤真菌棘孢曲霉(Aspergillus aculeatus)中分离得到2个新化合物和2个已知化合物,采用质谱(MS)、一维核磁共振波谱(1D NMR)、异核多键相关谱(HMBC)、异核单量子相关谱(HSQC)和旋转坐标NOE谱(ROESY)等方法对化合物的结构进行了鉴定,化合物2的顺反构型通过ROESY数据进一步确定.鉴定结果表明,2个新化合物分别为2-(2'-4'-6'-三羟基)-7-羟基-5-甲基色原酮{2-(2',4',6'-trihydroxyphenyl)-(7-hydroxy-5-methyl)chromone}(1)和(E)-4-羟基-3-[(3-甲基-4-羟基-2-丁烯)氧代]苯甲酸{(E)-4-hydroxy-3-[(4-hydroxy-3-methylbut-2-en-1-yl)oxy]benzoic acid}(2);2个已知化合物分别为(S)-2-[(2'-羟基)丙基]-5-甲基-7-羟基色原酮{2-(2'-hydroxypropyl)-5-methyl-7-hydroxychromone}(3)和(3R,4S)-8-羟基-3,4,5-三甲基-6酮-4,6-二氢-3H-异色烯-7-羧酸{(3R,4S)-8-hydroxy-3,4,5-trimethyl-6-oxo-4,6-dihydro-3H-isochromene-7-carboxylic acid}(4).活性测试结果表明,这4个化合物均表现出一定的抗氧化活性.     

银-组氨酸配合物-蒙脱石抗菌剂的制备及抗菌活性

以银-组氨酸配位阳离子[Ag(His)]⁺为前驱体, 采用水热离子交换法制备了抗变色耐盐性的新型银-组氨酸配合物-蒙脱石抗菌剂(SHMMT). 用电感耦合等离子体发射光谱仪(ICP)测定了抗菌剂的载银量, 用X射线衍射仪(XRD)和热重-差热分析仪(TG-DTA)表征了抗菌剂的结构, 用平板计数法测试了SHMMT对交替假单胞菌(Pseudoalteromonas carrageenovora)的抗菌活性, 通过海水浸泡实验对抗菌剂的耐盐性和缓释性进行了测试. 结果表明, 当组氨酸与Ag⁺的摩尔比为1:1时, SHMMT抗菌剂的载银量高达1.7 mmol/g, 远大于蒙脱石(Na-MMT)的阳离子交换容量. 该产品为白色粉末, 具有很强的抗变色能力和抗菌活性. SHMMT在海水中浸泡45 d后杀菌率仍达80%, 耐盐性和缓释性良好, 是一种用途广泛的环保型抗菌材料.     

常用中药藁本中新化合物的结构, 合成及活性研究

藁本是常用中药。中国药典收录的藁本有两种植物: 中国藁本(Ligusticumsinense Oliv. )和辽藁本(L. jeholense Thell), 另外新疆藁本(Conioselinumvaginatum Thell)做为藁本代用品在新疆地区广泛应用。我们对三种藁本植物中的化学成分进行深入研究, 从中共分到30种单体化合物并进行结构鉴定, 其中4种新化合物。初步药理实验发现从新疆藁本中分到的几个化合物具明显降酶保肝活性; 从中国蒿本中分到的蒿本酚显示较强的免疫抑制活性, 为探讨构效关系,作者完成了这些具活性成分的合成研究, 并合成一些结构类似物, 详细的活性研究还在进行中。     

几个新的席夫碱合铜(Ⅱ)配合物的合成及性质研究

有关席夫碱类配体及配合物的合成研究非常多,Padhye S.等曾概括过变更席夫碱配合物活性方式^[1],β－二酮席夫碱形成的金属配合物具有仿酶催化活性,在仿生研究中有重要意义;此外,氨基酸类席夫碱含有多个强电负性配位原子,具有较强的配位能力和多样的配位模式的优点,因此,我们合成结构较为复杂的氨基酸席夫碱及其与生命金属铜（II）的配合物,并对合成的配合物的抗菌活性进行了初步研究。     

硼烷簇合物的结构规则

从超额电子数出发，提出了1种稠合型硼烷的结构规则，讨论了各种规则间的关系。     

Syntheses,crystal structures and thermodecomposition behaviors of three energetic compounds

Three new energetic compounds, nickel(II) 3,5-dinitro-2-pyridonate (Ni(2DNPO)₂(H₂O)₄, 1), copper(II) 3,5-dinitro-4-pyridonate (Cu(4DNPO)₂(H₂O)₄, 2) and cobalt(II) 3,5-dinitro-4-pyridone-N-hydroxylate ([Co(4DNPOH)₂(H₂O)₄] · 2DMF, 3 · 2DMF), were characterized by elemental analysis, FT–IR, TG-DSC and X-ray single crystal diffraction analysis. Complexes 1 and 2 are similar in structure with the metal ion coordinated by oxygen donors of four water molecules on the equatorial position and two nitrogen donors of the pyridone rings of two ligands in the axial positions. The cobalt(II) complex 3 · 2DMF is a heavily distorted octahedral geometry. The Co(II) has equatorial positions defined by oxygens of four water molecules. Its axial positions are filled with two oxygen atoms of the pyridone-N-hydroxylate of two ligands. The TG-DSC results reveal that 1 is the most stable, with higher initial thermal decomposition temperature and enthalpy. Based on the thermoanalyses, the nickel compound is a promising candidate as a component in catalyzed RDX-CMDB propellants in comparison with our earlier lead(II) analogs.     

Modulation of antibiotic activity by the hydroalcoholic extract from leaves of Caryocar coriaceum WITTM

The aim of this study was to identify the presence of tannins, phenols and flavonoids on the hydroalcoholic extract of Caryocar coriaceum leaves (HECCL) and to determine the antioxidant and antibacterial activity of this extract. The extract was tested alone (1024–1 μg/mL) or associated (MIC/8) with several antibiotics in order to identify any antibacterial activity against multiresistant bacterial strains (Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa). The existence of tannins, total phenols (901.31 mg/g) and flavonoids (89.68 mg/g) was confirmed in the HECCL. The presence of rutin and quercetin were confirmed by Thin-layer chromatography (TLC). Using the 2,2-diphenyl-1-picrylhydrazyl (DPPH) method, the antioxidant activity of the extract (9 μg/mL) was determined. Moreover, the Minimum Inhibitory Concentration (MIC) value found for HECCL was 1024 μg/mL and the association between HECCL (MIC/8) with benzylpenicillin significantly changed its minimum inhibitory concentration from 2500 to 625 μg/mL against E. coli.     

新型层柱化合物合成、表征及催化活性

将含过氧铌一、三取代钨硅、钨磷过氧杂多阴离子利用离子交换法嵌入Zn2Al类水滑石中制得层柱化合物,利用XRD,IR,UV等方法对产物的结构进行了表征。结果表明在层柱化合物中过氧杂多阴离子仍然保持Keggin结构,并且过氧键没被破坏。层柱化合物在酯化反应中显示优良的催化性能。     

Synthesis of novel azabicyclo derivatives containing a thiazole moiety and their biological activity against pine-wood nematodes

Abstract

To explore a new skeleton with nematicidal activity, a series of novel azabicyclo derivatives containing a thiazole moiety were designed, synthesized and evaluated for their nematicidal activities. The bioassay results against pine-wood nematodes (Bursaphelenchus xylophilus) showed that most of the title compounds displayed nematicidal activity at a concentration of 40?mg/L. Especially, the title compounds2-((8-methyl-8-azabicyclo[3.2.1]octan-3-yl)oxy)-4-(4-chlorophenyl)thiazole (7e), 2-((8-methyl-8-azabicyclo[3.2.1]octan-3-yl)thio)-4-phenylthiazole (10a) and 2-((8-methyl-8-azabicyclo [3.2.1]octan-3-yl)thio)-4-(4-chlorophenyl)thiazole (10e) exhibited more than 90% mortality against Bursaphelenchus xylophilus.     

Crystal structure and magnetic properties of two bimetallic chain compounds

Two bimetallic magnetic chain compounds of {[Mn(dpop)(H₂O)][Mn(dpop)][Fe[CN]₆]•8.5H₂O•0.5DMSO} _n ( 1 ) and {[Mn(dpop)][Ni[CN]₄]} _n ( 2 ) (dpop = 2,13-dimethyl-3,6,9,12,18-pentaazabicyclo-[12.3.1]-octadeca-1(18),2,12,14,16-pentaene) have been synthesized and characterized by single-crystal X-ray diffraction and magnetic measurements. Both complexes have cyano-bridged chain structures, in which complex 1 is a zigzag chain, while complex 2 is nearly a straight line. The magnetic susceptibility results indicate that there is a weak ferromagnetic interaction between manganese (II) ions in complex 1 , whereas the interaction is antiferromagnetic in complex 2 .     

Synthesis,structure, ADME and biological activity of three 2,6-disubstituted thiosemicarbazone derivatives

Three new 2,6-disubstituted thiosemicarbazone derivatives of pyridine, namely, 2-{amino[6-(pyrrolidin-1-yl)pyridin-2-yl]methylidene}-N,N-dimethylhydrazine-1-carbothioamide, C₁₃H₂₀N₆S, 2-{amino[6-(piperidin-1-yl)pyridin-2-yl]methylidene}-N,N-dimethylhydrazine-1-carbothioamide, C₁₄H₂₂N₆S, and 2-[amino(6-phenoxypyridin-2-yl)methylidene]-N,N-dimethylhydrazine-1-carbothioamide monohydrate, C₁₅H₁₇N₅OS·H₂O, have been synthesized and characterized by NMR spectroscopy and low-temperature single-crystal X-ray diffraction. In addition, their antibacterial and anti-yeast activities have been determined. The ability of the tested compounds to inhibit bacterial growth was comparable to vancomycin as a reference drug. Compared to isoniazid (MIC 0.125 and 8 µg ml⁻¹), the compounds showed the ability to inhibit the growth of Mycobacterium tuberculosis to a moderate degree for the standard strain and at the same level or higher (MIC 4–8 µg ml⁻¹) for the resistant strain. All three compounds adopt the zwitterionic form in the crystal structure regardless of the presence or absence of solvent molecules.     

Synthesis of novel chiral compounds of purine and pyrimidine bases

The physiologically active groups such as purine and pyrimidine bases are introduced to the asymmetric ynthesis. The optically pure compounds bearing purine and pyrimidine bases (5a—5e) were prepared via the asymetric Michael addition reaction of purines and pyrimidines as Michael donators with the chiral source 5-(R)-[(1R, 2S, 5R)-menthyloxy]-2(5H)-furanone (3a), which was prepared from the natural chiral auxiliary (-)-menthol. The synthetic method was studied in detail and the new compounds were identified on the basis of their analytical data and spectroscopic data, such as [α]_D~(20), IR, UV, ~1H NMR, ~(13)C NMR and MS. The absolute configuration of 5a was established by X-ray crystallography. The results provided an efficient synthetic route to chiral purines and pyrimidine analogues, and offered chiral sources for further research on the physiologically active compounds of chiral nucleotides.     

Microwave synthesis,structure, and properties of molybdophosphate compounds

Two compounds of disphosphopentamolybdate(VI) with the formulae (C₄H₁₄N₂O)₃- [P₂Mo₅O₂₃]?·?3H₂O (1) and (C₄H₁₄N₂O)₅(NH₄)₂[P₂Mo₅O₂₃]₂?·?5H₂O (2) have been synthesized by a simple, fast and efficient microwave method, and their crystal structures and spectroscopic properties have been studied. The heteropoly anion [P₂Mo₅O₂₃]^6? has a known structure built of five MoO₆ octahedra and two PO₄ tetrahedra. The MoO₆ octahedra form a pentagonal ring by sharing four edges and one corner and the PO₄ tetrahedra are attached to one side of the ring by three oxygen atoms. The most interesting feature of compound 1 is its extensive framework based on a one-dimensional zigzag chain. In compound 2, a more extensive and complicated framework of hydrogen bonds joins the anions, organic cations and water molecules together.     

Identification of Cyclic Dipeptides and a New Compound (6-(5-Hydroxy-6-methylheptyl)-5,6-dihydro-2H-pyran-2-one) Produced by Streptomyces fungicidicus against Alternaria solani

As an important microbial resource, Actinomycetes, especially Streptomyces, have important application values in medicine and biotechnology. Streptomyces fungicidicus SYH3 was isolated from soil samples in tomato-growing areas and showed good inhibitory effects on Alternaria solani in tomato. To obtain pure active compounds, SYH3 fermentation broth was subjected to XAD-16 macroporous resin and silica gel column chromatography. Combined with the repeated preparation and separation of preparative high-performance liquid chromatography (HPLC), a total of four monomer compounds were obtained after activity tracking. Compound 4 was identified as a new six-membered lactone ring compound named 6-(5-hydroxy-6-methylheptyl)-5,6-dihydro-2H-pyran-2-one by 1D and 2D nuclear magnetic resonance (NMR) data and mass spectrometry (MS). The other three active compounds belong to the cyclodipeptide, and their half maximal inhibitory concentration (IC₅₀) values against A. solani were 43.4, 42.9, and 30.6 μg/mL, respectively. Compound 4 significantly inhibited the spore germination and induced swollen and deformed local hyphae of A. solani with an IC₅₀ value of 24.9 μg/mL. Compound 4 also had broad-spectrum antifungal activity and had a good antifungal effect on the tested plant-pathogenic fungi. The modes of action of new compound (4) still require further investigation, representing a novel and effective anti-fungal agent for future application.