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291.
[reaction: see text] A facile and efficient synthetic route toward highly substituted 2,3-dihydrothiopyran-4-ones 2 has been developed via a formal [5C + 1S] annulation of readily available alpha-alkenoyl ketene-(S,S)-acetals 1 with sodium sulfide nonahydrated salt (Na2S x 9H2O) and utilized in the synthesis of 2-(4-chlorophenyl)-6-(morpholin-4-yl)-4H-thiopyran-4-one 5l, an inhibitor of DNA-dependent protein kinase (DNA-PK). 相似文献
292.
二溴羟基苯基荧光酮—乳化剂OP荧光熄灭法测定微量铬(Ⅵ) 总被引:11,自引:3,他引:11
本文基于Cr(Ⅵ)-二溴羟基苯基荧光酮(DBH-PF)-OP体系的荧光熄灭效应,提出一种测定痕量铬(Ⅵ)的新荧光方法。在pH2.4-4.1的HCl-NaAc缓冲介质和OP存在下,Cr(Ⅵ)与DBH-PF形成1:2的橙红色络合物,络合物的最大激发发工和发射波长分别是365mm和528nm。铬(Ⅵ)量在0.05-1.5μg/25ml范围内与△F呈线性关系,检测限是2.0ng/ml。方法用于电镀废液,废 相似文献
293.
Lee JS Kim DH Liu KH Oh TK Lee CH 《Rapid communications in mass spectrometry : RCM》2005,19(23):3539-3548
Searchable MS/MS spectra libraries, constructed using the results of liquid chromatography coupled with electrospray ionization (ESI) tandem mass spectrometry (LC/MS/MS) with data-dependent acquisition on an ion trap mass spectrometer, are presented with regard to the identification and confirmation of a variety of closely related flavonoids in a set of biological samples. Flavonoids were found to exhibit a maximum amount of structurally specific MS/MS spectra at 45% of normalized collision energy on the instrument used, without wideband activation. These MS/MS spectra were then searched automatically against a 297-substance MS/MS library that contains many previously acquired spectra of standard flavonoids. The possible applications of this powerful technique to biological samples are also discussed. Daidzein and genistein were identified through the MS/MS spectra library while searching through LC/MS/MS data for plant and microbial extracts. Moreover, these compounds proved completely distinguishable from other flavonoids of closely related structures in the MS/MS spectra library, using the NIST MS search program. The applicability of the library-searchable spectra at low concentrations was demonstrated by successful identification of daidzein and genistein at 0.05 and 0.5 microg/mL, respectively. 相似文献
294.
羧基丙烯酸酯涂料合成及其防雾性能研究 总被引:3,自引:2,他引:3
采用种子乳液聚合法合成了一种互穿网络型羧基丙烯酸酯类聚物乳液,研究了加料方式对羧基分布的影响,结果表明丙烯酸加入到核单体中有利于羧基分布在乳胶粒表面。在体系中引入离子键交联结构提高了乳液涂料的硬度和耐水性能,离子键交联PILN型涂料具有优良的防雾性能。 相似文献
295.
We have used the high nucleophilicity of bromide ion in the form of the ionic liquid, 1-n-butyl-3-methylimidazolium bromide ([bmim][Br]), for the nucleophilic displacement of an alkyl group to regenerate a phenol from the corresponding aryl alkyl ether. Using 2-methoxynaphthalene (1) as a model compound, we found that the combination of ionic liquid [bmim][Br] and p-toluenesulfonic acid with warming effected demethylation in 14 h, affording the desired product 2-naphthol (2) in good yield (97%). Various other protic acids (MsOH, hydrochloric acid (35%), dilute sulfuric acid (50%)) could be used as a proton source in this demethylation reaction. Under the same conditions, cleavage of alkyl alkyl ether 2-(3-methoxypropyl)naphthalene yielded mixture of corresponding 2-(3-bromopropyl)naphthalene and 2-(3-hydroxypropyl)naphthalene. Dealkylation of various aryl alkyl ethers could also be achieved using significantly reduced (i.e., stoichiometric) amounts of concentrated hydrobromic acid (47%) in the ionic liquid. Both procedures afforded the desired products in moderate to good yield; however, cleavage of aryl alkyl cyclic ether, 2,3-dihydrobenzofuran, resulted in low yield of the desired product o-2-bromoethylphenol. The convenience of this method for ether cleavage and its effectiveness using only a moderate excess of hydrobromic acid make it attractive as a green chemical method. 相似文献
296.
A novel vanadium(IV) phosphite, (VO)(4)(4,4'-bpy)(2)(HPO(3))(4), was hydrothermally synthesized and characterized by single-crystal X-ray diffraction. This compound crystallizes in the monoclinic system with the space group C2/c and cell parameters a = 35.970(3) A, b = 15.9400(13) A, c = 10.7681(7) A, beta = 101.073(4) degrees, and Z = 8 with R(1) = 0.0482. The structure of the compound consists of trigonal bipyramidal [VO(4)N] and pseudopyramidal [HPO(3)] blocks, which are connected by corner-sharing, to form vanadium phosphite layers in the bc plane. These layers are further linked through 4,4'-bpy pillars, generating a 3D framework. Thermogravimetric analysis and magnetic susceptibility data for this compound are given. 相似文献
297.
The interaction of fluorocarbon containing hydrophobically modified polyelectrolyte(FMPAANa) with two kinds of nonionic surfactants(hydrogenated and fluorinated)in a semidilute (0.5wt%) aqueous solution had been studied by rheological measurements,Association behavior was found in both systems.The hydrophobic interaction of FMPAANa with fluorinated surfactant(FC171) is much stronger than that with hydrogenated surfactant(NP7.5) at low surfactoant concentrations.The interaction is strengthened by surfactants being added for the density of active junctions increased.Whereas distinct phenomena for FC171 and NP7.5 start to be found as the surfactants added over their respective certain concentration.The interaction of polyelectrolyte with fluorinated surfactant increases dramatical ly while that with hydrogenated surfactant decreases. 相似文献
298.
The B3LYP and MP2 methods with 6-31G* basis set were used to predict the geometries of N, N-dimethylformamide (DMF) dimer and DMF–aromatic hydrocarbons interaction systems. A total of 10 conformers were obtained with
no imaginary frequencies, respectively. The interaction energies of these binary mixtures have been obtained. The analyses
of chelpg charge distribution and the atoms in molecules theory (AIM) were used to analyze the nature of the interaction.
The results show the presence of hydrogen bonds between DMF and aromatic hydrocarbons. The interaction between DMF and benzonitrile
is the strongest with the interaction energy of −21.58 kJ mol−1 (BSSE corrected), and the intensity order of interactions is DMF–benzonitrile: d2 > DMF–DMF: a2 > DMF–toluene: c1 > DMF–benzene:
b2. 相似文献
299.
Jin‐Yu Sun Zhen Zhao Yong‐Chao Ma Miao‐Li Zhu Xiang‐Dong Zhang 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(1):m4-m6
The crystal structure of the title compound, μ‐2‐hydroxybutanedioato‐1κ2O4,O4′:2κ3O1,O2,O4‐nitrato‐2κO‐tris(1,10‐phenanthroline)‐1κ4N,N′;2κ2N,N′‐dicopper(II) nitrate tetrahydrate, [Cu2(C4H3O5)(NO3)(C12H8N2)3](NO3)·4H2O, contains an unsymmetrical dinuclear copper complex with Cu(phen)2 and Cu(phen)(NO3) moieties (phen is 1,10‐phenanthroline) bridged by a malate (2‐hydroxybutanedioate) ligand, which acts as a double‐bridging and tetradentate ligand. As a result of this double‐bridging action, especially the direct coordination of the O atom of one carboxylate group of malate to the two Cu atoms, the Cu⋯Cu distance is only 4.199 (1) Å and the two phen planes are roughly parallel [the shortest interplanar distance is 3.28 (1) Å], exhibiting an obvious intramolecular π–π stacking interaction. 相似文献
300.
A new class of M(II)–Hg(II) (M=Cu(II), Co(II), Ni(II)) mixed-metal coordination polymers, Cu(2-pyrazinecarboxylate)2HgCl2 (4), [Co(2-pyrazinecarboxylate)2(HgCl2)2] · 0.61H2O (5) and [Ni(2-pyrazinecarboxylate)2(HgCl2)2] · 0.77H2O (6), have been prepared by self assembly of metal-containing building blocks, M(2-pyrazinecarboxylate)2 · (H2O)2(M=Cu(II), Co(II), Ni(II)), with HgCl2. Compounds 4–6 were characterized fully by IR, elemental analysis and single crystal X-ray diffraction. Compound 4 crystallized in the monoclinic space group C2/c, with a=17.916(5) Å, b=7.223(2) Å, c=13.335(4) Å, β=128.726(3)°, V=1346.2(6) Å3, Z=4. It contains alternating Hg(II) and Cu(II) metal centers that are cross-linked by 2-pyrazinecarboxylate spacers and chlorine co-ligands to generate a unique three-dimensional Hg(II)–Cu(II) mixed metal framework. Compound 5 crystallized in the triclinic space group P
, with a=6.3879(7) Å, b=6.6626(8) Å, c=13.2286(15) Å, α=96.339(2)°, β=91.590(2)°, γ=113.462(2)°, V=511.71(10) Å3, Z=1. Compound 6 also crystallized in the triclinic space group P
, with a=6.3543(8) Å, b=6.6194(8) Å, c=13.2801(16) Å, α=96.449(2)°, β=92.263(2)°, γ=113.541(2)°, V=506.67(11) Å3, Z=1. Compounds 5 and 6 are isostructural and in the solid state the Hg(II)M(II)Hg(II) units are connected by Hg2Cl2 linkages to produce a novel M(II)–Hg(II) (M=Co(II), Ni(II)) zigzag mixed-metal chain, in which a new type of M–M′–M′–M array was observed. The metal containing building blocks, M(2-pyrazinecarboxylate)2 · (H2O)2 (M=Cu(II), Co(II), Ni(II)), exhibit different connectivities to HgCl2 depending on the metal cation contained within them. 相似文献