Organotin Polyesters and Polyethers — Synthesis and Biocidal Properties

Poly-tributyl and -triphenyltin esters or ethers were prepared by reaction of various natural and synthetic polymers containing carboxyl, sulfonic or hydroxyl groups with organotin chlorides, hydroxides or oxides. The biocidal properties of the polymers were investigated.     

Synthesis and Characterization of Water-Soluble Metal Binding Polyesters Containing Pendant Carboxylic Moiety

The water-soluble polyesters were synthesized by the polyaddition reaction between diethylenetriaminepentaacetic acid bisanhydride (DTPABA) and polyethylene glycols (PEG) of different molar masses. The copper complexes of these polyesters were synthesized by the reaction with copper acetate and were characterized by their melting points, elemental analyses, viscometry, FT-IR, UV-visible SEM, AFM, XRD data. Thermal stability of the compounds was studied by TG-DTA analyses. The antibacterial activity of the polyesters was studied against the bacterial species E. coli, S. aureus, P. aeruginosa and B. subtilis. All the polyesters showed moderate anti-bacterial activity against the selected bacteria.     

羧酸和乙酸酐合成甲基酮的研究

酮是化学化工行业应用广泛的重要中间体,其常见的合成方法这些年来不断有新的报道。文章研究了以常见的羧酸和乙酸酐为起始原料合成甲基酮的方法。该方法实施简单,产物收率62%～89%,为酮提供了一种未见文献报道的合成新方法。     

金刚烷甲酸纤维素酯的合成与表征

以N,N-二甲基乙酰胺/LiCl为溶剂,以对甲苯磺酰氯为共反应剂原位活化金刚烷甲酸,在均相反应体系中合成了新的纤维素高级脂肪酸酯——金刚烷甲酸纤维素酯。采用红外光谱、核磁共振谱进行了表征。热重分析表明,在纤维素链中引入金刚烷基可提高其热稳定性,取代度越高,热稳定性越好。金刚烷甲酸纤维素酯在有机溶剂中的溶解性随取代度增大而提高。     

Synthesis and Characterization of Organotin Polyesters Derived from 3,5-Pyridinedicarboxylic Acid

Organotin polyesters were synthesized from the interfacial condensation of organotin dihalides and salts of 3,5-pyridinedicarboxylic acid. The polymers are synthesized in moderate to high yields and are moderate to high polymers. MALDI MS, IR spectral, and NMR spectral results are consistent with the proposed structure. The Sn–O stretching band is found at about 1,028 cm^?1. Infrared spectra are consistent with majority of the products having a non-bridged structure about the tin. All of the polymers exhibit some inhibition of two pancreatic cancer cell lines. The dibutyltin and dicyclohexyltin products show sufficiently good inhibition of both cell lines as to merit further testing.     

Microwave-Assisted Synthesis and Characterization of Stearic Acid Sucrose Ester: A Bio-Based Surfactant

Sugar esters of fatty acids are bio-based surfactants that were synthesized by transesterification of table sugar (sucrose) with stearic acid methyl ester (SAME) in high yield and purity using an optimized microwave-assisted method. The maximum surfactant product yield of 88.2% was obtained by combining reactants with potassium methoxide and irradiating the mixture with microwaves to achieve an ideal reaction temperature of 132 °C over 21 min. The synthetic procedure described herein minimized undesirable sugar pyrolysis as evidenced by retention of white color characteristic of a pure bio-based surfactant product. The experiment implemented Box–Behnken design for response surface methodology to refine reaction parameters for optimal product yield. The following parameters were augmented: the irradiation time, the mole ratio of catalyst to sucrose, and temperature.     

三嗪含硫羧酸金属配合物的合成及性质表征

以三聚硫氰酸为母体,与氯乙酸反应得到了具有三个羧基的柔性羧酸配体2,2',2″-[1,3,5-三嗪-2,4,6-三(硫代)]三乙酸(H_3TTTA),利用该配体分别与过渡金属盐反应得到了六种配合物,对配体和配合物分别进行~1H-NMR、元素分析、IR、TG的表征,推测了配合物的结构。这为后期三嗪含硫羧酸金属配合物在功能材料、生命科学等领域的应用研究提供理论基础。     

Synthesis and Properties of Novel Surface Active Monomers Based on Derivatives of 4‐Hydroxybutyric Acid and 6‐Hydroxyhexanoic Acid

Novel surface active maleate and methacrylate monomers based on derivatives of ω‐hydroxy carboxylic acids have been synthesized. The monomers are comprised of hydrophobic alkyl chains and hydrophilic poly(ethylene glycol), quaternary ammonium, sulfonate and carboxylic fragments. Synthesized monomers sufficiently reduce surface tension at the aqueous solution‐air interface. The copolymerization of synthesized monomers with 5‐tert‐butylperoxy‐5‐methyl‐2‐hexene‐3‐yne monomer and N‐vinylpyrrolidone in solvent and emulsion copolymerization of synthesized peroxide containing surface active monomer with styrene have been carried out. The synthesized surface active monomers have been shown to be suitable emulsifiers for obtaining polystyrene colloid dispersions. It has been ascertained that the surface active copolymers obtained can form stable interpolyelectrolyte complexes with oppositely charged polymers.     

Centratherun ritchiei Seed Oil — Characterization of Vernolic Acid

Vernolic acid has been found at the 30.1% level in Centratherum ritchiei (Compositae) seed oil. This acid, cis-12, 13-epoxyoctadec-cis-9-enoic, was isolated by preparative TLC and characterized by IR, NMR and MS. A successful attempt has been made to identify vernolic acid, without its derivatization, by mass spectral study. A reference vernolic acid (Vernonia anthelmintica seed oil) has been used for comparison purpose throughout the study.     

Synthesis and Structural and Initial Cancer Cell Line Characterization of Organotin Polyesters from Dipicolinic Acid

The interfacial polymerization is employed to produce high polymer poly(ester ethers) from the reaction of the salt of dipicolinic acid and various organotin dihalides. They are rapidly synthesized with yield increasing as the length of the organotin alkyl chain increases. Infrared spectroscopy shows the formation of new bands derived from the Sn–O and Sn–O(CO) linkages. IR also shows that the products exist as a combination of molecular geometries about the tin atom. MALDI MS shows formation of ion fragment clusters to five and six units in length. The products show good inhibition of a variety of cancer cell lines including two pancreatic cancer cell lines.     

手性羧酸铑的合成及应用研究

手性羧酸铑盐作为重要的金属催化剂,在重氮化合物参与的手性控制以及活性控制反应中扮演着重要的角色。文章主要在已有文献报道的背景下,对手性羧酸铑盐的合成路线做了进一步改进探究。     

3-氯-6-环丙烷基-8-三氟甲基咪唑[1,2-a]吡啶-2-甲酸的合成与表征

以2-氨基-3-三氟甲基吡啶为原料,通过NBS选择性溴化,再与溴代丙酮酸甲酯通过"一锅法"进行烷基化环化反应,之后经选择性氯化、Suzuki偶联反应和水解,合成了咪唑并[1,2-a]吡啶甲酸衍生物——3-氯-6-环丙烷基-8-三氟甲基咪唑并[1,2-a]吡啶-2-甲酸。反应总收率达到36.5%。并对Suzuki偶联反应的催化剂和反应条件进行了探讨。     

Synthesis,Characterization and Electrical Conductivity of Polyesters Containing Azomethine Linkages

Abstract

The synthesis and characterization of some polyesters containing azomethine linkages are reported here. The electrical conductivity of these polyesters is measured and the results are explained with simple Pariser-Parr-Pople calculations. The polymers are doped with Ag and the electrical conductivity of most of the doped polymers is found to register significant increase. Attempts are made to explain this increase in electrical conductivity.     

蔗糖酯的合成与应用研究进展

蔗糖酯是一种性能优良的非离子表面活性剂,综述了蔗糖酯的合成方法,分别了溶剂法（包括二甲基甲酰胺法、丙二醇法、水溶剂法、甲醇法及相转移催化法）及非溶剂法（包括生物合成法）。对蔗糖酯的应用及市场情况作了较为详细的介绍。     

Synthesis,Characterization and Evaluation of Surface and Thermal Properties of 3‐Cyclohexyloxy‐2‐Hydroxypropyl Pyridinium and Imidazolium Surface‐Active Ionic Liquids

In this work, 1‐halo‐3‐(cyclohexyloxy)propan‐2‐ol ( 3a/3b ) were reacted with N‐methylimidazole ( 4 ) or pyridine ( 5 ) to yield the respective 3‐(3‐(cyclohexyloxy)‐2‐hydroxypropyl)‐1‐methyl‐1H‐imidazol‐3‐ium ( 6a/6b ) or pyridinium ( 7a/7b ) surface‐active ionic liquids (SAIL). The self‐aggregation behavior of these ionic liquids (IL) was evaluated by conductometric and tensiometric methods. The thermal stability and size of the micelles were determined by thermogravimetric analysis and dynamic light scattering studies, respectively. The investigated IL were found to exhibit very low cytotoxicity as evaluated by MTT (3‐(4, 5‐dimethylthiazol‐2‐yl)‐2, 5‐diphenyltetrazolium bromide) assay on the C6 glioma cell line, indicating that the investigated SAIL can be considered for biological applications like drug and gene delivery. The conventional IL 3‐methyl‐1‐octyl imidazolium bromide ( C ₈ mimBr ) was used for comparison in property evaluations.     

生理活性氨基酸Schiff碱的合成与表征

用天冬酰胺分别与水杨醛、邻香草醛、2 ,4 二羟基苯甲醛在甲醇中反应 ,然后加入异丙醇析出产物的方法合成了三种氨基酸Schiff碱 ,产物收率分别为 84 3 %、81 2 %、76 7%。用元素分析、红外光谱、紫外光谱等手段对所合成的Schiff碱进行了表征。采用EPR技术对所合成的Schiff碱清除超氧阴离子自由基 (O2 ·)的性能进行了研究 ,结果表明 ,所合成的氨基酸Schiff碱质量浓度为 5kg/m3 时 ,对O2 ·的清除率分别达到 6 3 4%、6 2 .0 %、84 2 % ,具有明显的生理活性。     

基于羧酸功能化离子液体的含铽发光材料的合成与表征

合成了两种带羧酸官能团的长链咪唑离子液体,离子交换前后分别溶解稀土氧化铽,得到新型的荧光软材料,荧光光谱及荧光寿命表征显示离子液体配体与稀土离子之间进行了有效的能量传递,此荧光材料兼具稀土离子的优异荧光特性和离子液体本身的性质,有较高的潜在应用价值.     

Synthesis and Characterization of a New Class of Energetic Compounds – Ammonium Nitriminotetrazolates

1‐Methyl‐5‐nitriminotetrazole ( 1 ) and 2‐methyl‐5‐nitraminotetrazole ( 2 ) obtained by nitration of 1‐methyl‐5‐aminotetrazole ( 3 ) and 2‐methyl‐5‐aminotetrazole ( 4 ) were deprotonated using aqueous ammonia solution yielding the energetic compounds, ammonium 1‐methyl‐5‐nitriminotetrazolate ( 5 ) and ammonium 2‐methyl‐5‐nitriminotetrazolate ( 6 ). The nitrogen‐rich salts were tested and characterized comprehensively using vibrational spectroscopy (Infrared (IR) and Raman), multinuclear (¹H, ¹³C, ¹⁴N, and ¹⁵N) NMR spectroscopy, and elemental analysis. The molecular structures in the crystalline state were determined using low temperature single crystal X‐ray diffraction. The thermal behavior and the decompositions were investigated using differential scanning calorimetry (DSC) and gas IR spectroscopy. The heats of formation were calculated using bomb calorimetric measurements. In addition, the relevant detonation parameters, like the detonation pressure and velocity of detonation were calculated using the software EXPLO5 outperforming the values of TNT. Last but not least the sensitivities were determined using BAM methods showing moderate values against impact and friction (drophammer and friction tester) and the long‐term stabilities were tested using Flexy Thermal safety calorimetry (TSC). X‐ray crystallography: 5 : monoclinic, P2₁/c, a=370.06(2) pm, b=2079.06(9) pm, c=859.69(5) pm, β=99.120(5)°, V=65306(6) pm³, Z=4, ρ_calc=1.639 g cm⁻³; 6 : monoclinic, P2₁, a=365.39(2) pm, b= 788.82(5) pm, c=1124.95(7) pm, β=91.818(6), V=32408(3) pm³, Z=2, ρ_calc=1.651 g cm⁻³.     

含邻氨基苯甲酸新型三核席夫碱化合物的合成与表征

以邻氨基苯甲酸、3-羧基水杨醛、乙酸铜和乙酸锌为原料合成了新型Cu2+、Zn2+三核席夫碱配合物。以氯仿和无水乙醇做溶剂,在pH7~8的条件下顺利合成得到了新型Cu2+、Zn2+三核席夫碱配合物,并对它们的合成条件分别进行了探索性实验,确定了合成它们的各自优化条件。产品通过元素分析1、H NMRI、R、UV和MS进行组成和结构表征。     

磺酸磁性石墨烯固体酸的制备、表征及初步应用研究

以氧化石墨烯,Co（NO3）2·6H2O和Fe（NO3）3·9H2O为离子源利用水热法一步制备磁性石墨烯（Co Fe2O4-h GO）,用磺酸重氮盐将其重氮化制得磺酸磁性石墨烯固体酸,采用FT-IR、XRD、VSM和酸碱反滴定法测对其进行了表征。结果表明,链接石墨烯的Co Fe2O4为单相立方尖晶石结构,平均粒径为27 nm,饱和比磁化强度MS为29.7 A·m2/kg,其表面酸量为2.7 mmol/g。用乙酸与正己醇的酯化反应初步评估其催化性能：在90℃,乙酸与正丁醇摩尔比为1∶1,催化剂用量为3wt%,反应时间为4 h的条件下,乙酸转化率为59.1%。