共查询到20条相似文献,搜索用时 62 毫秒
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以苯基-3,5-二(甲氧基羰基)-2-异(口恶)唑啉-N-氧化物为偶极体,丙烯酸乙酯为亲偶极体,通过[3+2]环加成反应,简便地合成了含有多官能团的1-氮杂-2,8-二氧杂二环[3.3.0]-辛烷类化合物。该反应条件温和,产率较高(50%~93%).化合物的结构经元素分析,1H NMR,13C NMR,IR和MS确认和表证,并对其波谱性质进行了讨论。 相似文献
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为克服目前合成方法存在收率较低,反应时间长、产品分离困难等不足,本文以β-D-葡萄糖、乙酰溴为原料,经乙酰化、溴代反应合成了糖基体2,3,4,6-O-四乙酰基-α-D-溴代葡萄糖,再与4-羟基苯甲醛衍生物经糖苷化反应合成了5种4-甲酰基苯基(2,3,4,6-O-四乙酰基)-β-D-葡萄糖苷衍生物。 在合成4-甲酰基苯基(2,3,4,6-O-四乙酰基)-β-D-葡萄糖苷衍生物的过程中,采用10%(质量分数)NaOH溶液为缚酸剂,三(3,6-二氧杂庚基)胺(TDA-1)为相转移催化剂,反应物的收率为61%~69%,并应用核磁共振技术确定了产品的结构。 该方法具有产品收率较高,反应温和、操作简单等优点。 相似文献
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InCl3 was found to be a mild and effective catalyst for the simple and efficient synthesis of spiro-perimidine derivatives by the reaction of naphthalene-1,8-diamine and active carbonyl compounds in water at room temperature. This protocol includes some important aspects like the use of water as a “green” reaction medium, good yielding of products and mild reaction conditions. 相似文献
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Suprava Nayak Gouri S. BrahmaK. Venugopal Reddy K. Veera ReddyAnadi C. Dash 《Polyhedron》2011,30(10):1637-1645
The oxidation of glyoxylic acid (HGl) by MnIVL {L4− = tetra deprotonated 1,8-bis(2-hydroxybenzamido)-3,6-diazaoctane} was investigated in the pH range 1.67-10.18, at 25-45 °C and 0.5 M ionic strength. The reaction exhibited biphasic kinetics with MnIIIL− as the reactive intermediate. MnIV was reduced to MnII. The products of oxidation of HGl were identified as formic acid and CO2 in acidic medium, and oxalate in basic medium, consistent with the stoichiometry: −Δ[MnIV]/−Δ[HGl] = 1. In acidic medium, both MnIVL and MnIIIL− formed outer-sphere adducts with the neutral HGl {HC(OH)2COOH} molecule, with an association constant Qav of 28 and 70 M−1, respectively. A similar adduct formation was not observed for the glyoxylate mono anion {Gl−, CH(OH)2(CO2−)} and glyoxylate dianion {Gl2−, CH(OH)(O−)CO2−}. The rate and activation parameters for the various paths are reported and an outer-sphere electron transfer mechanism is suggested. 相似文献
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《Journal of Coordination Chemistry》2012,65(2):161-167
Abstract Several cobalt(III) complexes incorporating 2,2′-diaminobiphenyl(dabp) and other 2(2N)- or 4N-type ligands were prepared and resolved by chemical and chromatographic methods: (1) [Co(en)2(dabp)]Cl22H2O, (2) [Co(l-pn)2(dabp)] (ClO4)34H2O, (3) [Co(l-chxn)2(dabp)](ClO4)33H2O, (4) α-[Co(trien)(dabp)](ClO4)3, (5) α-[Co(2S,9S-dimetrien)(dabp)] (ClO4)3 2H2O, (6) α-[Co(3S,8S-dimetrien)(dabp)] (ClO4)33H2O, (7 [Co(tren)(dabp)]Cl35H2O, (8) [Co(bpy)2(dabp)] Cl33H2O. The complexes (1), (4) and (8) gave one pair of enantiomers, Δ(Λ) and Λ(δ), and the complexes (2) and (3) gave only one Δ-isomer. The absolute configuration of the complexes (5) and (6) was found to be Λ, and that of (7) was not determined because of unsuccessful resolution. The three geometric isomers of the complex (2) were separated and their structures assigned. 相似文献
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A straightforward and highly efficient series of new substituted 3-aryl-1,8-naphthyridine derivatives 3a–e, 4a–e, and 6a–e were synthesized. Condensation dissimilar quantities of 2-chloro-3-aryl-1,8-naphthyridine 1a–e with benzene-1,4-diamine 2 and sodium ethoxide refluxing in ethanol solvent yielded the compounds 3a–e and 4a–e. The 2-(4-((3-aryl-1,8-naphthyridin-2-yl)amino)phenyl)isoindoline-1,3-diones 6a–e were obtained by treatment of compounds 3a–e with phthalic anhydride 5 in refluxing N,N-dimethylformamide is described. All synthesized compounds evaluated for their antimicrobial activity. The structures of the compounds have been proven on the established of spectral (IR, 1H NMR, and 13C NMR) data and elemental analyses. The reaction will be characterized by good efficacy, easy workup, simple purification of the products, and availability of catalyst. 相似文献
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合成了新的单核三价钴化合物[Co(L)]NO3.2EtOH(H2L为2-羟基萘醛双缩三乙烯四胺),并借助元素分析、红外光谱和X射线单晶衍射对其结构进行了表征。单晶结构解析结果表明:标题化合物中三价钴离子与配体L2-2个氧原子及4个氮原子形成六配位结构。抗菌实验表明,配合物对真菌白色念珠菌,大肠杆菌,白菜软腐病菌,枯草杆菌,菜豆荤疫菌具有较高的生物活性。 相似文献
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Twelve compounds each having a six membered Si-contained heterocycle, have been successfully synthesized. Of these eleven compounds have never been reported in the literature. The structures were confirmed by Spectral analysis and elementary analysis. The stability and properties of these compounds is also discussed. 相似文献
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Summary 3,6-Dichloro- and 3,6-dibromo-8-quinolinols were prepared by direct halogenation of 8-nitroquinoline by N-halosuccinimide in acetic acid or by halogenation of the corresponding 6-halo-8-nitroquinoline prepared via aSkraup reaction. The nitro group was reduced to amino and the amine was hydrolyzed to the phenol in 70% sulfuric acid at 220°C. The fungitoxicity of 3,6-dichloro- and 3,6-dibromo-8-quinolinols, as well as intermediates in their preparation, againstAspergillus niger, Aspergillus oryzae, Myrothecium verrucaria, Trichoderma viride, andMucor cirinelloides was determined. 3,6-dichloro-8-quinolinol is the most fungitoxic analogue of this class of compounds observed to date.
Herstellung und Fungitoxizität von 3,6-Dichlor- und 3,6-Dibrom-8-chinolinen
Zusammenfassung 3,6-Dichlor- und 3,6-Dibrom-8-chinoline wurden durch direkte Halogenierung von 8-Nitrochinolin mit N-Halogensuccinimid in Essigsäure oder durch Halogenierung der entsprechenden nachSkraup synthetisierten 6-Halogen-8-nitrochinoline hergestellt. Die Nitrogruppe wurde zum Amin reduziert und die Aminofunktion in 70% iger Schwefelsäure bei 220°C zum Phenol hydrolysiert. Die Fungitoxizität der 3,6-Dichlor- und 3,6-Dibrom-8-chinoline und jene der bei ihrer Herstellung auftretenden Zwischenstufen gegenAspergillus niger, Aspergillus oryzae, Myrothecium verrucaria, Trichoderma viride undMucor cirinelloides wurde bestimmt. 3,6-Dichlor-8-chinolin ist der derzeit stärkste bekannte fungitoxische Vertreter dieser Substanzklasse.相似文献
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Xuefang Shang Jianmei Yuan Zhimin Du Yingling Wang Shenyu Jia Jie Han Yue Li Jinlian Zhang Xiufang Xu 《Helvetica chimica acta》2013,96(4):719-731
Three fluorescent turn‐on probes containing 3,6‐dichloro‐9H‐carbazole as carbazyl part have been designed and synthesized. Among studied anions F?, AcO?, H2PO , Cl?, Br? and I?, AcO? showed the strongest binding ability with all probes. The strong basic anions, such as AcO?, H2PO , and F?, induced a significant red‐shift in absorption and a concomitant increase in fluorescent emission of the probes caused by photoinduced electron transfer (PET). The determination limit of probe 3 (Scheme 1) toward AcO? is 3.0×10?7 M . 1H‐NMR Titration experiments shed light on the nature of the interaction between the probes and the anions. Theoretical investigation further illustrated the possible binding mode in these host? guest interactions and the roles of molecular frontier orbitals in molecular interplay. 相似文献
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《Journal of Coordination Chemistry》2012,65(1-2):97-108
Abstract The synthesis of the new ligand 1,8-bis(quinolyloxy)-3,6-dithiaoctane (1) and the corresponding Cu(II), Cu(I) and Co(II) complexes is reported. The crystal and molecular structure of the copper(II) complex, [Cu(1)](ClO4)2.3H2O, has been determined by X-ray diffraction methods. The complex crystallizes in the orthorhombic space group Fddd, with cell data Z = 16, a = 20.326(2), b = 20.879(3) and c = 28.308(4)Å. The structure consists of discrete [Cu(1)]?2+ cations separated by (structurally disordered) perchlorate anions and three lattice water molecules per cation. The coordination geometry about the copper atom is pseudo-octahedral with the quinoline nitrogen and thioether sulfur atoms at the equatorial positions and the ether oxygen atoms at the axial positions. 1H NMR line-broadening experiments indicate that electron-transfer self-exchange reactions between the copper(I) and copper(II) complexes of (1) is immeasurably slow on the NMR time-scale. The coordination chemistry of (1) is compared with its oxygen analogue, 1,8-bis(quinolyloxy)-3,6-dioxaoctane. 相似文献
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A novel chromogenic reagent, 2-(2-sulfo-4-acetylphenylazo)-7-(2,4,6-trichlorophenylazo)-1,8-dihydroxynaphthalene-3,6-disulfonic acid 1, was prepared by diazo coupling of 4-acetylaniline-2-sulfonic acid and 2,4,6-trichloroaniline to chromotropic acid through –N=N– groups. Based on this reagent, a simple, sensitive and selective spectrophotometric method was developed for the determination of lead. In 0.20M phosphoric acid medium, lead reacts with 1 to form a 1:2 blue complex with an absorption maximum of 654nm. Beers law is obeyed in the range of 0–0.6mgL–1 of lead. The apparent molar absorptivity is 1.25×105Lmol–1cm–1. The detection limit and quantification limit were found to be 0.63µgL–1 and 2.1µgL–1, respectively. The relative standard deviation for eleven replicate measurements was of 2.6%. The interference of foreign ions was also investigated. All the other foreign ions studied did not interfere with lead determination except for Ca(II) and Ba(II). The interference caused by Ca(II) and Ba(II) can be eliminated by prior extraction of lead with potassium iodide-methylisobutylketone (KI-MIBK). The proposed method was applied to the determination of lead in certified samples with satisfactory results. 相似文献