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51.
52.
Reaction of β-naphthyl cinnamate with anhydrous aluminum chloride afforded 9-hydroxyphenalenone5 by a Fries rearrangement followed bya dearylative cyclisation. 9-Hydroxy-3-phenyl-2,3-dihydrophenaIen-l-one7 was identified as an intermediate. 相似文献
53.
Baeza A Nájera C Sansano JM Saá JM 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(13):3849-3862
The enantioselective synthesis of cyanohydrin O‐phosphates by using in situ generated bifunctional catalysts (R)‐ or (S)‐3,3′‐bis(diethylaminomethyl)‐1,1′‐binaphthol–aluminium chloride (binolam–AlCl) is reported. The reaction, which can be described as an overall cyano‐O‐phosphorylation of aldehydes, has a wide scope and applicability. Evidence is also provided, including ab initio and DFT calculations, in support of supported by the Lewis acid/Brønsted base (LABB) dual role of the catalyst in inducing first the key enantioselective hydrocyanation, which is then followed by O‐phosphorylation. A brief screening of the synthetic usefulness of the resulting cyanohydrin O‐phosphates unveiles some interesting applications. Among them, chemoselective hydrolysis, reduction and palladium‐catalysed nucleophilic allyl substitution, thereby leading to enantiomerically enriched α‐O‐phosphorylated α‐hydroxy esters, β‐amino alcohols and γ‐cyanoallyl alcohols, respectively. Naturally occurring (?)‐tembamide and (?)‐aegeline are synthesised accordingly. 相似文献
54.
Luminescentmaterialshavinglongdecayperi0dhaveat-IIactedmuchinterestduetotheirpotentialwidespreadaPplicati0ns.Recently,alongdecayluminescentp0wderhavingthecomPositionofSrAl2O4activatedwithEu' wasreportedandregardedasthebestcandidateforpracticalaPPlicationbecauseofitsuniqueadVantages0veritsprecursors.l'2Inthispaper,wereportthesynthesisofthelongdecayluminescentpowderandtheinnuence0fthemolarratioofAlt0sr0ntheethessioncolor.Toproducethelundnescentp0wder,amixtureofSrCO3,Al2O3,Eu2O3andsomesol… 相似文献
55.
B. M. Bulychev V. N. Verbetskii A. I. Sizov T. M. Zvukova V. K. Genchel’ V. N. Fokin 《Russian Chemical Bulletin》2007,56(7):1305-1312
Crystallization of non-solvated aluminum hydride from a diethyl ether-benzene mixed solvent was studied. The desolvation of
AlH3·(Et2O)x etherate in solution and the crystallization of α-AlH3 during polythermal heating of the solution occur only in the presence of ≥10 wt.% LiAlH4. The process is multistage, and the crystallization begins with the formation of the AlH3·0.25Et2O solvate, which recrystallizes in the solid phase into γ-AlH3 and then α-AlH3. Four crystalline modifications of aluminum hydride were characterized by X-ray diffraction and electron microscopy.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1259–1265, July, 2007. 相似文献
56.
合成了两个酰腙类荧光探针1和2,在DMSO-H_2O(7∶3,体积比)体系中,两者分别在478 nm和460 nm处对Al~(3+)具有较好的荧光选择识别作用。Job's法、核磁滴定、质谱分析表明,探针1和2与Al~(3+)的配位比均为1∶2,且对Al~(3+)的检出限分别为9.58×10~(-8) mol/L和6.52×10~(-8) mol/L。同时提出了探针1和2对Al~(3+)的荧光传感机理。实际应用研究表明,探针1和2可用于河水和自来水中一定浓度范围内Al~(3+)的检测。 相似文献
57.
Preconcentration Systems Using Polyurethane Foam/Me-BDBD for Determination of Copper in Food Samples
Valfredo Azevedo Lemos Daniel Rodrigues Vieira Cleber Galvão Novaes Marcelo Eça Rocha Moacy Selis Santos Regina Terumi Yamaki 《Mikrochimica acta》2006,153(3-4):193-201
A new reagent, 6-[2′-(6′-methyl-benzothiazolylazo)]-1,2-dihydroxy-3,5-benzenedisulfonic acid (Me-BDBD), was synthesised and
used in on-line and off-line systems for copper preconcentration by solid-phase extraction. Spectrophotometry and Flame Atomic
Absorption Spectrometry (FAAS) were the detection techniques. Polyurethane foam loaded with Me-BDBD packed in a minicolumn
was used as sorbent in both systems. The spectral characteristics of Me-BDBD were investigated. The optimum pH values for
maximum sorption of the metal are between 7.0 and 8.5. Copper was desorbed with 0.05 and 0.50 mol L−1 hydrochloric acid solutions, for on-line and off-line systems, respectively. The effects of several foreign substances on
the adsorption of copper are reported. The enrichment factors obtained were 7 (on-line) and 26 (off-line) for the systems.
The proposed procedures allowed the determination of copper with detection limits of 3.4 and 1.4 μg L−1 (0.85 and 0.35 μg per gram of sample) for on-line and off-line systems, respectively. The precision of the procedures was
also calculated: 3.2 (on-line) and 1.9% (off-line). The validation of the procedures was carried out by analysis of certified
reference material. The copper contents in corn and rice flour and black tea samples were determined by applying the proposed
procedures. 相似文献
58.
《Electroanalysis》2003,15(17):1397-1402
A new analytical procedure for the simultaneous determination of aluminum(III) and iron(II) in two kinds of dialysis fluids (peritoneal and hemodialysis fluids) by differential pulse adsorptive stripping voltammetry (DPAdSV) is described. The voltammetric measurements were performed using, as working electrode, a stationary mercury electrode, and a platinum electrode and a Ag|AgCl|KCl(sat.) electrode as auxiliary and reference electrodes, respectively, employing acetate buffer solutions at different pH as supporting electrolyte. As complexing agents, Solochrome Violet RS, Palatine Chrome Black 6BN, Chromazurol S and Eriochrome Black T were employed. For both elements, the accuracy, expressed as relative recovery R%, was very satisfactory being in the range 94–105%, the precision as repeatability, expressed as relative standard deviation sr%, was lower than 6%, while the limits of detection were of the order of a few units of μg/L. The analytical voltammetric procedure has been validated by comparison with spectroscopic (graphite furnace atomic absorption spectroscopy, GFAAS) measurements. 相似文献
59.
Various aluminum alkoxide precursors have been used for the preparation of boehmite by hydrothermal assisted sol-gel processing. The coordination status of aluminum in solution for all precursors employed for the preparation of boehmite phase was determined by 27Al NMR and correlation between coordination status of aluminum atoms of precursors and development of boehmite phase has been investigated. Hydrothermal assisted hydrolysis of aluminum alkoxides where the aluminum atoms are four or five coordinated in solution resulted in the formation of boehmite. In contrast, hydrothermal hydrolysis of aluminum alkoxides where the aluminum atoms are six coordinated resulted in the formation of amorphous gel. Development of boehmite phase by hydrothermal hydrolysis of aluminum alkoxides at various temperatures was pursued by X-ray diffraction (XRD) and Fourier Transform Infrared (FTIR) spectroscopy. 相似文献
60.
The sorption behaviour of 2.5 × 10−5 M solution of Cd(II) on polyurethane foam (PUF) from iodide medium have been investigated. The conditions were optimized from aqueous solutions of different pH (1-10) and of acids of varied concentration (0.01-1.0 M). The maximum concentration of KI was found to be 0.24 M and equilibration time was established to be 20 min. The data successfully followed the Freundlich and Dubinin-Radushkevich (D-R) isotherms at low metal ion concentration while Langmuir isotherm followed at higher metal ion concentration. The Freundlich parameter 1/n = 0.66 ± 0.02 have been evaluated whereas D-R isotherm yields the sorption free energy E = 10.5 ± 0.1 kJ mol−1 indicating ion exchange type chemisorption. The monolayer coverage (XL) constant of Langmuir isotherm was found to be 23.7 ± 0.4 mg g−1. The numerical values of thermodynamics parameters enthalpy (ΔH), entropy (ΔS) and Gibbs free energy (ΔG) indicated the endothermic and spontaneous nature of sorption. The Scatchard plot analysis was tested to evaluate the binding sites of the PUF and stability constants of sorption were determined. On the basis of these parameters, the sorption mechanism was discussed. Among the foreign ions tested, Pb(II), Hg(II), cyanide and nitrite should be absent. The clean separation of Cd(II) from Zn(II) ions in the ratio 1:250, respectively, was achieved by column chromatography. 相似文献