Synthesis and characterization of novel derivatives of triazinone

Triazinone is a kind of heterocyclic compound with potential biological activity. The molecular design, synthesis and optimization of lead compounds are important to the development of insecticides. Six new triazinone derivatives were synthesized and characterized by IR, ¹H-NMR and MS spectra. The mechanism of synthesis of aminotriazinone was discussed. Translated from Huaxue Tongbao (Chemistry), 2006, 69(9): 674–679 (in Chinese)     

含全氟烷基磺酰基新型异黄酮化合物的合成

异黄酮类化合物广泛存在于植物中,是许多中草药的有效成分。美国食品和药物管理局将大豆列为能够真正降低患心脏病危险的少数食品之一,研究发现大豆防病作用的关键因素在于其中大量存在的各类黄酮类成分[1]。1993年Coward等[2]首次报道大豆异黄酮具有抵御癌细胞的作用,其后W ei     

Synthesis and characterization of poly(amideimide)s containing pendent flexible alkoxy chains

A series of aromatic diacylhydrazides containing pendent flexible alkoxy chains, viz., 5-butyloxyisophthalicacid dihydrazide, 5-octyloxyisophthalicacid dihydrazide, 5-dodecyloxyisophthalicacid dihydrazide and 5-hexadecyloxyisophthalicacid dihydrazide were synthesized by the hydrazinolysis reaction of the corresponding aromatic esters with hydrazine hydrate. Diacylhydrazides were each polycondensed with aromatic dianhydrides, viz., 4,4′-oxydiphthalic anhydride (ODPA), 3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA) and pyromellitic dianhydride (PMDA) to obtain new poly(amideimide)s. Poly(amideimide)s had inherent viscosity in the range 0.55-0.88 dL/g in N,N-dimethylacetamide (DMAc) at 30 ± 0.1 °C. Poly(amideimide)s were found to be soluble in DMAc, N,N-dimethylformamide (DMF), 1-methyl-2-pyrrolidinone (NMP) and pyridine and could be cast into tough, flexible and transparent films from a solution in DMAc. X-ray diffractograms revealed that poly(amideimide)s with longer alkoxy chains had layered structures. Glass transition temperature of poly(amideimide)s containing pendent flexible alkoxy chains were in the range 215-245 °C. Temperature at 10% weight loss was in the range 380-410 °C in nitrogen atmosphere indicating good thermal stability of poly(amideimide)s.     

Synthesis and Photovoltaic Properties of Formyl End-Capped Oligothiophenes

For the purpose of developing novel photovoltaic materials, 5,5″-biformyl-2,2′:5′,2″-terthiophene (OHC-3T-CHO) and 5,5″″-biformyl-2,2′:5′,2″:5″,2″′:5″′,2″″-q-uinquethiophene (OHC-5T-CHO) were synthesized. The photovoltaic properties of OHC-3T-CHO and OHC-5T-CHO were studied. We have fabricated two flexible organic photovoltaic devices using OHC-3T-CHO, OHC-5T-CHO, and 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA). The PET-ITO (indium tin oxides coated with polyethylene terephthalate)/OHC-3T-CHO/PTCDA/Al device has an open circuit voltage (V _oc ) of 1.12 V, and photoelectric conversion efficiency (PCE) of 1.00%, whereas the PET-ITO/OHC-5T-CHO/PTCDA/Al device has a V _oc of 1.78 V and PCE of 1.08%. Both devices have high V _oc (1.12 V and 1.78 V). It is possible that intermolecular hydrogen bonding between the –CHO group of OHC-nT-CHO and the carboxylic dianhydride of PTCDA enhanced the efficiency by promoting forward interfacial electron transfer.     

一种新型呋喃香豆素类似物: 呋喃并萘并吡喃酮的合成及DNA嵌入活性

1,5-萘二酚经Pechmann缩合，烯丙基醚化，Claisen重排，乙酰化，溴加成，闭环六步反应，合成了一个新型的呋喃香豆素类似物，2H-4,8-二甲基呋喃并[2',3':5,6]萘并[1,2-b]吡喃-2-酮(6)。所得2～6的5个新化合物的结构均经^1H NMR，MS，IR，元素分析确证，测试了化合物6的紫外及荧光光谱。在DMSO-Tris HCl体系中，用荧光淬灭技术考察了6和7的DNA嵌入活性，求取了Scatchard表观嵌入常数，发现6和7都能有效地嵌入小牛胸腺DNA中，6的嵌入活性小于7。     

新型低聚噻吩衍生物的设计、合成及其液晶性能的研究

设计、合成了一系列新型低聚噻吩衍生物N,N’-双烷烃基-5,5’-二溴基-2 ,2’：5’,2’-三噻吩-4,4’-二酰胺[N,N’-dialkyl-5,5’-dibromo-2,2’:5 ’,2’-terthiophene-4,4’-dicarboxamide](DNCnDBr3T,n=5,8,6,18)。示差扫描 量热法（DSC）测定的结果及偏光光学显微镜观察的结果显示,DNC18DBr3T, DNC16DBr3T,DNC8DBr3T具有近晶A形液晶性质,DNC5DBr3T不具有液晶性质。为了探 讨分子间氢链对液晶形成的影响,设计、合成了新型低聚噻衍生物4,4“-双烷烃 酯-5,5“-二溴基-2,2’:5’,2’-三噻吩[4,4’-bis(alkyloxycarbonyl)-5,5’ -dibromo-2,2’:5’,2’-terthiophene](DOCnDBr3T,n=5,8,16,18).测定和观察的 结果发现,DOCnDBr3T(n=5,8,16,18）不具有液晶的结果。这个结果表明,酰胺基 的存在于液晶的形成起着重要的作用。测定DNC18DBr3T在结晶状态和液晶状态下的 红外光谱,进一步证实了部分分子间氢键对于液晶的形成起着重要的作用。     

硫杂蒽酮的合成和表征

为了寻求合成硫杂蒽酮的高效新方法,以2,2′-二硫代二苯甲酸和苯酚为原料,硫酸为溶剂和催化剂,考察了沸石分子筛、Al2O3和P2O5、温度、原料的物质的量之比、反应时间对反应收率的影响,确定了最佳反应条件,推测了可能的反应过程;进而以2,2′-二硫代二苯甲酸和相应的苯衍生物为原料,在H2SO4-P2O5体系中于最佳反应条件下制备了13个硫杂蒽酮类化合物,并利用柱色谱分离以及红外光谱与核磁共振谱对产物进行表征.结果表明,在反应体系中引入P2O5有利于促进反应的完成;最佳反应条件为:温度70℃、2,2′-二硫代二苯甲酸/苯衍生物物质的量之比1∶6、反应时间6h.邻苯二酚与二硫代水杨酸的反应产物——化合物11(a)和11(b)为同分异构体.     

Synthesis and characterization of novel chiral diporphyrins and their dimetal complexes

Reaction of chiral 2,2'-biamino-1,1'-binaphthalene (R or 5) with monosubstituted porphyrin 1b and 2b-c afforded novel chiral diporphyrins 3a-c and 4a-c. Their dimetal complexes [(M)2DiPor] have also been prepared. Both structures have been identified by MS, IR, UV-visible, 1H NMR spectra and elemental analysis. These novel chiral compounds show very high optical activities.     

Synthesis and Structure of [Cu（OH）2（H2O）2（4—C5H4N—COOH）2]

1 INTRODUCTION Supramolecular chemistry and crystal engineering of coordination compounds have attracted considerable interests nowadays owing to the fascinating structural diversity and potential applications as functional materials[1,2]. Generally, architectures of supramolecules are formed through hydrogen bonds, ?- ?stacking interaction or other weak interactions between the molecules. Recently, many supramolecular compounds containing silver(I) and copper(II) species have been re-…     

Synthesis and characterization of boron nitride sponges as a novel support for metal nanoparticles

This paper describes a simple synthetic route for the synthesis of hexagonal boron nitride (h-BN) powders with high specific surface area, in which BBr3, NH4Cl and Al powders are used as starting materials. The structure and composition of the powders were characterized by electron diffraction, Fourier transformation infrared spectroscopy and X-ray photoelectron spectroscopy in the selected area. X-ray diffraction shows wide peaks of crystalline h-BN with the particle size on the nanometer scale, and transmission electron microscopy reveals that the products have a novel spongy morphology. Silver nanoparticles loaded h-BN sponges were prepared via a one-step synthesis method. Different reaction conditions for the formation of h-BN sponges were also investigated.     

新型腰果酚双子表面活性剂的合成及表面活性

以天然生物质腰果酚、1,3-二溴丙烷及氯磺酸为原料,通过醚化、磺化及中和三步反应合成了一类新型的腰果酚基磺酸盐双子(Gemini)表面活性剂.采用傅立叶转换红外光谱仪和核磁共振谱仪表征了产物的结构;采用滴体积法测定了腰果酚Gemini表面活性剂的表面张力,研究了水溶液的表面性质,并与相应的单基腰果酚基磺酸盐表面活性剂进行了对比.结果表明:腰果酚Gemini表面活性剂水溶液的临界胶束浓度(cmc)为6.20×10-2 mmol.L-1,远小于相应的单基腰果酚表面活性剂水溶液的cmc(8.40mmol.L-1);其临界表面张力γcmc为36.92mN.m-1,与单基腰果酚表面活性剂水溶液的相近(γcmc为38.41mN.m-1).与此同时,腰果酚Gemini表面活性剂水溶液的最小分子截面积Amin为0.27nm2,比相应的单基表面活性剂水溶液的小得多.     

一种低代超支化聚醚的合成、表征及表面活性研究

以十二胺、丙烯酸甲酯和乙二胺为原料,甲醇为溶剂,采用发散合成法合成一种低代超支化分子骨架.采用1H NMR对分子骨架的结构进行了表征.在此基础上,以低代骨架为起始剂,分别与环氧乙烷、环氧丙烷加成制备了一种超支化聚醚,测定了它的表面张力、浊点,同时计算出了它的HLB值.结果表明:骨架的分子结构与所设计的结构相符,合成的聚醚具有典型表面活性剂的性质.     

吴茱萸碱的合成及其结构表征和体内抗肿瘤作用

以色胺和N-甲基靛红酸酐作为起始原料合成了吴茱萸碱;利用元素分析仪、红外光谱仪、核磁共振谱仪、质谱仪等对合成产物进行了结构表征,并研究了其对小鼠移植性肉瘤S180和小鼠肝癌H22的体内抗肿瘤作用.结果表明,所合成的吴茱萸碱在高、中、低剂量(20 mg·kg-1、10 mg·kg-1、5 mg·kg-1)下均对S180和...     

Synthesis and characterization of model polyether-ester ionomers

In this study, a series of polyether-ester ionomers was prepared by neutralizing the carboxylic acid groups in 1 : 1 copolymers of benzenetracarboxylic dianhydride (BTDA) and poly(tetramethylene oxide) or poly(ethylene oxide) glycol. The base polymers were in a liquid state while the ionomers were in solid state and a separate ionic phase was formed. The local structure and the morphology of the ionomers were investigated by dynamic mechanical analysis, Fourier transform infrared spectroscopy, and small-angle x-ray scattering as well as extended x-ray absorption fine structure. Clearly, the geometric structure of the ionic sites varied with the nature of the metal ions and the morphology of the ionomers was determined by the microstructure of the ion aggregates. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 799–806, 1997     

Synthesis and characterization of novel polybenzimidazoles bearing pendant phenoxyamine groups

A novel aromatic diacid, 3, 5‐dicarboxyl‐4′‐amino diphenyl ether, containing pendant phenoxy amine group was synthesized. Homo‐ and co‐polybenzimidazoles containing different content of pendant phenoxyamine groups were synthesized by condensation of 3,3′‐diaminobenzidine with this acid and a mixture of this acid and isophthalic acid in different ratio in polyphosphoric acid. Copolybenzimidazoles with structural variations were also synthesized based on this acid and pyridine dicarboxylic acid, terephthalic acid, adipic acid, or sebacic acid. The polymers have good solubility in polar aprotic solvents and strong acids and they form tough flexible films by solution casting. The polymers were characterized by different instrumental techniques (FTIR, TGA, DSC, XRD, etc.) and for solvent solubility, mechanical properties, inherent viscosity, and proton conductivity. The inherent viscosities of the polymers vary in the range of 0.62–1.52 dL/g. They have high thermal stability up to 475–506 °C (IDT) in nitrogen, high glass transition temperatures (T_g) ranging from 313 to 435 °C and good tensile strength ranging from 58 to 125 MPa. Proton conductivity of homo polymer is 3.72 × 10^?3 S/cm at 25 °C and 2.45 × 10^?2 S/cm at 200 °C © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 5776–5793, 2008     

Alumina-titania oxides: Synthesis and characterization

Alumina-titania mixed oxides with nominal atomic ratios Al/Ti=25 and 2 have been synthesized by cohydrolysis of Al(OsecBu)₃ and Ti(OBu)₄. The oxides were amorphous at 500°C, showing only short range order. Ti was incorporated in alumina in a well dispersed way creating a true Al/Ti mixed oxide. The strength of surface acid sites and specific surface areas were increased at the higher Ti content. The TiO₂ anatase phase was avoided and rutile was formed directly at 900°C.     

Liquid crystalline behaviour of hydrazide derivatives containing alkoxyazobenzene

Two series of dissymmetric hydrazide derivatives containing alkoxyazobenzene with nitro terminal group and octyloxy terminal group, N-4-alkoxyphenyl-N′-4-((4-nitrophenyl)azophenyl) benzohydrazide (Bn-NO₂, n indicates the number of carbon atoms) and N-4-octyloxyphenyl-N′-4-((4-octyloxyphenyl)azophenyl) benzohydrazide (B8-B8), were designed and synthesised, and their liquid crystalline properties were investigated by means of differential scanning calorimetry, polarised optical microscopy and wide-angle X-ray diffraction. It was found that B8-B8 with octyloxy terminal chains displayed monolayer smectic C phase, whereas Bn-NO₂ with nitro terminal group displayed SmA_d phase, and intermolecular hydrogen bonding was confirmed as the driving force. In addition, the effect of hydrogen bonding, dipole–dipole interactions and steric hindrance effect on the liquid crystalline structures were also discussed.     

Synthesis,characterization, crystal structure,and antimicrobial studies of novel thiourea derivative ligands and their platinum complexes

N,N-Di-R-N′-(4-chlorobenzoyl)thiourea (Di-R: diethyl, di-n-propyl, di-n-butyl and diphenyl) ligands (HL^1–4) and their Pt(II) complexes (cis-[Pt(L^1–4-S,O)₂]) have been synthesized and structurally characterized by elemental analyses, FT-IR and NMR spectroscopy. HL² ligand and cis-[Pt(L⁴-S,O)₂] metal complex have been also characterized by a single-crystal X-ray diffraction study. HL², C₁₄H₁₉ClN₂OS, crystallizes in the monoclinic space group P2₁/n (no. 14), with Z = 4, and unit cell parameters, a = 11.1405(16) Å, b = 9.7015(12) Å, c = 14.790(2) Å, β = 106.547(7)°. The cis-[Pt(L⁴-S,O)₂], C₄₀H₂₈Cl₂N₄O₂PtS₂: triclinic, space group P-1 (no. 2), a = 8.9919(3) Å, b = 14.7159(6) Å, c = 15.7954(6) Å, α = 113.9317(18)°, β = 97.4490(18)°, and γ = 105.0492(16)°. Single crystal analysis of complex, cis-[Pt(L^1–4-S,O)₂], revealed that a square planar coordination geometry is formed around the platinum atom by two sulfur and two oxygen atoms of the related ligands, which are in a cis configuration. In addition, the thiourea derivative ligands and their complexes were evaluated for both their in-vitro antibacterial and antifungal activity. The results have been reported, explained, and compared with fluconazole and ampicillin, used as reference drugs.     

Synthesis and Crystal Structure of a New Complex （H3IDC）（Prz）0.5（H2O）

The compound （H3IDC）（Prz）0.5（H2O） （H3IDC = imidazole-4,5-dicarboxylate, Prz = piperazine） has been prepared from a hydrothermal approach and was characterized by IR analysis and X-ray diffraction. Its crystal structure consists of discrete 4,5-imidazole-dicarboxylate, H2O and piperazine molecules. The whole structural motif was assembled by three different non-covalent interactions of O-H…O, N-H…O and π-π stacking, which play an important role in packing the molecules. Interestingly, the connections between imidazole-4,5-dicarboxylate molecule and water molecule result in a helical polymeric chain. Crystal data for compound 1： monoclinic system, space group P21/c, a = 6.4600（13）, b = 19.910（4）, c = 6.9123（14） A^°, β = 94.26（3）°, V= 886.6（3） A^°^3, Z= 4, C7H10O5N3, Mr = 216.18.