- Metal-Urea Complex - A Precursor to Metal Nitrides
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A novel and general route to synthesize various metal nitrides (AlN, CrN, and ζ-Fe2N) from metal-urea complexes is presented. These complexes, especially metal-urea chloride, have proved to be useful precursors to metal nitrides, because urea molecules construct a coordination sphere around the metal atom and form a stable structure, compared with the air-sensitive halide. Different anions in the second coordination sphere determine the reaction mechanism. The transformation from metal-urea chloride to nitride is thought to follow a nucleation-growth mechanism, while that from metal-urea nitrate is thought to follow a nitridation mechanism. We anticipate that this metal-urea complex will find applications in the fabrication of other, more complex, nitrides.
- Qiu, Yu,Gao, Lian
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- Equilibrium and structure of the Al(III)-ethylenediamine-N,N′-bis(3- hydroxy-2-propionate) (EDBHP) complex. A multi-method study by potentiometry, NMR, ESI MS and X-ray diffraction
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The equilibrium and structure of the complex formed by Al(iii) and ethylenediamine-N,N′-bis(3-hydroxy-2-propionate) (EDBHP2-) have been studied using pH-potentiometry, 1H and 27Al NMR, ESI MS and single crystal X-ray diffraction methods. The EDBHP ligand is a strong Al-binder in aqueous solution for pH between 4 and 8 and for cAl = cEDBHP ≥ 0.1 mmol dm-3. The dominating complex identified by ESI MS and potentiometry is a neutral dimer, Al2L 2(OH)2, with logβ22-2 = 14.16 ± 0.03. In the solid Al2(EDBHP)2(OH)2· 2H2O the Al(iii) ions are connected through a double hydroxo bridge. Both four-dentate organic ligands are coordinated terminally through two carboxylate groups and two N-donors forming three five-membered chelate rings. The hydroxyl groups of the ligand EDBHP remain protonated and are not coordinated to the aluminium ions. The structure and composition of the dimer are very likely the same in solution and the solid state. The Royal Society of Chemistry 2006.
- Joszai, Robert,Kerekes, Imola,Satoshi, Igarashi,Sawada, Kiyoshi,Zekany, Laszlo,Toth, Imre
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- ETHYL-SUBSTITUTED (η5-CYCLOPENTADIENYL)-BIS(DIHALOALANEDI-μ-HALO)TITANIUM(III) AND (η6-BENZENE)BIS(DIHALOALANEDI-μ-HALO)TITANIUM(II) CHLORO AND BROMO COMPLEXES
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Ethyl-substituted trinuclear complexes CpTiAl2Cl8-xEtx (x=1-4) were prepared by the reaction of CpTiCl3 with two equivalents of ethylaluminium compounds.The complexes were characterized by the half-width of their EPR single-line spectra, which decreased f
- Mach, Karel,Antropiusova, Helena,Polacek, Jindrich
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- Behavior of UO2 in a room-temperature ionic liquid in the presence of AlCl3
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A study was made of interaction between AlCl3 and room-temperature ionic liquid (RTIL) [C8H15N 2][N(SO2CF3)2], or BuEtIm-Tf 2N, and of anodic dissolution in RTIL of UO2 and of a simulated oxide fuel at 297-302 K, depending on the AlCl3 concentration. It was shown that anodic dissolution of UO2 pellets and a UO2-Al mixture in RTIL yields soluble uranium species. Potentiostatic electrolysis of the resulting solutions can yield uranium compounds at the cathode, though with low current efficiencies. The role of AlCl3 in these processes was suggested. A heterophase reaction between UO2 and AlCl3 was studied, depending on the content of AlCl3 in solution. It was found that the exchange reaction products, soluble uranium species, are accumulated in solution only at the molar ratio AlCl3/Tf2N > 1.
- Smolenskii,Bove,Borodina,Bychkov,Osipenko
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- Radiochemical Investigation of Thulium Chloride-Aluminium Chloride and Gadolinium Chloride-Aluminium Chloride Vapor Complexes
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The vapour pressures of complex species of the systems GdCl3/AlCl3 and TmCl3/AlCl3 were investigated by radiochemical analysis.The composition as well as the enthalpies and entropies of formation of the complexes were calculated.
- Steidl, G.,Baechmann, K.,Dienstbach, F.
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- Use of 1,4-bis(2,2,6,6-tetramethyl-1-oxyl-4-piperidyl)butane as a probe for studying acid sites
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ESR spectroscopy was applied to study paramagnetic complexes of the nitroxyl biradical of 1,4-bis(2,2,6,6-tetramethyl-1-oxyl-4-piperidyl)butane formed with AlCl3 in a toluene solution and resulted from the interaction with the acid sites on the SiO2 and γ-Al 2O3 surface. This biradical in solution forms a complex with two AlCl3 molecules, and a complex with two hydroxyl groups is formed on the SiO2 surface. When the biradical is adsorbed on the γ-Al2O3 surface, complex formation is complicated because of steric hindrance preventing bidentate coordination. Springer Science+Business Media, Inc. 2007.
- Fionov,Sadykov
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- Speciation in the AlCl3/SO2Cl2 catholyte system
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The fundamental chemical behavior of the AlCl3/SO 2Cl2 catholyte system was investigated using 27Al NMR spectroscopy, Raman spectroscopy, and single-crystal X-ray diffraction. Three major Al-containing species were found to be present in this catholyte system, where the ratio of each was dependent upon aging time, concentration, and/or storage temperature. The first species was identified as [Cl2Al(μ-Cl)]2 in equilibrium with AlCl3. The second species results from the decomposition of SO2Cl 2 which forms Cl2(g) and SO2(g). The SO 2(g) is readily consumed in the presence of AlCl3 to form the crystallographically characterized species [Cl2Al(μ-O 2SCl)]2 (1). For 1, each Al is tetrahedrally (T d) bound by two terminal Cl and two μ-O ligands whereas, the S is three-coordinated by two μ-O ligands and one terminal Cl. The third molecular species also has Td-coordinated Al metal centers but with increased oxygen coordination. Over time it was noted that a precipitate formed from the catholyte solutions. Raman spectroscopic studies show that this gel or precipitate has a component that was consistent with thionyl chloride. We have proposed a polymerization scheme that accounts for the precipitate formation. Further NMR studies indicate that the precipitate is in equilibrium with the solution.
- Boyle, Timothy J.,Andrews, Nicholas L.,Alam, Todd M.,Tallant, David R.,Rodriguez, Mark A.,Ingersoll, David
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- The standard enthalpies of formation of crystalline aluminium(III) bromide and aluminium(III) iodide
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The enthalpies of solution of crystalline AlCl3 and KBr were measured successively in one portion of 3.5 mol dm-3 HCl solution as well as AlBr3 and KCl in another.The measurements were carried out in a 100 cm3 reaction vessel of the isoperibol calorimeter LKB-8700.The standard enthalpy of the resuming reaction: AlCl3(c) + 3 KBr(c) = AlBr3(c) + 3 KCl(c), was found to be ΔH0r(298.15 K) = (63.4 +/- 1.3) kJ mol-1 which leads to ΔH0f(AlBr3, c, 298.15 K) = (-512.6 +/- 1.9) kJ mol-1.The same measurements were carried out for AlCl3 and KI and for AlI3 and KCl.The standard enthalpy of reaction: AlCl3(c) + 3 KI(c) = AlI3(c) + 3 KCl(c), was found to be ΔH0r(298.15 K) = (80.1 +/- 1.4) kJ mol-1 which leads to ΔH0f(AlI3, c, 298.15 K) = (-302.9 +/- 2.0) kJ mol-1.
- Efimov, M. E.,Kislova, G. N.,Medvedev, V. A.
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- Phase diagrams of some non-quasi-binary joins of the AlCl 3-BiCl3-NaCl system
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Phase diagrams of NaAlCl4-(70.0 mol % AlCl3 + 30.0 mol % BziCl3), NaAlCl4-(34.2 mol % AlCl3 + 65.8 mol % BiCl3), and (61.0 mol % AlCl3 + 39.0 mol % NaCl)-AlCl3 ? BiCl
- Kaloev,Turieva
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- AlN substrates: Fabrication via vapor phase growth and characterization
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A new vapor phase crystal growth technique was applied to fabricate single crystal AlN wafers up to 1.75-inch diameter. The wafers were sliced from AlN crystals and polished. Fabricated AlN wafers were investigated by X-ray diffraction, TEM, and cathodoluminescence. X-ray diffraction and TEM studies confirmed single crystal structure of grown material. High electrical resistivity of these AlN wafers was verified. AlN homoepitaxial layers exhibiting sharp near-band-edge emission were grown on fabricated AlN substrates. These results open the door for the commercialization of AlN substrates for advanced high-power mm-wave devices and optoelectronic devices based on Group III-nitride semiconductors.
- Melnik,Soukhoveev,Ivantsov,Sizov,Pechnikov,Tsvetkov,Kovalenkov,Dmitriev,Nikolaev,Kuznetsov,Silveira,Freitas Jr.
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- Synthesis in ionic liquids: [Bi2Te2Br](AlCl 4), a direct gap semiconductor with a cationic framework
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The Lewis acidic ionic liquid EMIMBr-AlCl3 (EMIM = 1-ethyl-3-methylimidazolium) allows a novel synthetic route to the semiconducting layered metal chalcogenides halide [Bi2Te 2Br]-(AlCl4) and its Sb analogue. [Bi2Te 2Br](AlCl4) is a direct band gap, strongly anisotropic semiconductor and consists of cationic infinite layers of [Bi2Te 2Br]+ and [AlCl4] anions inserted between the layers.
- Biswas, Kanishka,Zhang, Qichun,Chung, In,Song, Jung-Hwan,Androulakis, John,Freeman, Arthur J.,Kanatzidis, Mercouri G.
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- New luminescent terbium complex for the determination of DNA
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New terbium complexes of derivatives of 2-oxo-4-hydroxy-quinoline-3- carboxylic acid are reported, which are highly luminescent, water soluble and do not require luminescence enhancers. The triplet-state energy levels of the ligands, the relative quantum yields (QYs) and the excitation maxima of the respective terbium chelates were determined. The large luminescence enhancement of one of these complexes by nucleic acids was investigated and a mechanism of its interaction with DNA is proposed. The optimal conditions for determination of DNA are equal concentrations of Tb3+ and ligand R1 (C = 1 × 10-6 M), pH 9.0. Under optimal conditions the luminescence intensity (RI) is proportional to the concentration of fish sperm DNA (fsDNA) or calf thymus DNA (ctDNA), respectively, within the range of 0.05-1.5 μg ml-1. The detection limits were 10ng ml-1 for fsDNA and 12 ng mr-1 for ctDNA.
- Yegorova, Alla,Karasyov, Alexander,Duerkop, Axel,Ukrainets, Igor,Antonovich, Valery
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- Regioselective Synthesis of 1,5-Disubstituted 1,2,3-Triazoles by Reusable AlCl3 Immobilized on γ-Al2O3
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(Chemical Equation Presented) There is rapidly growing interest in the synthesis and use of substituted 1,2,3-triazoles. We report an easy and interesting procedure that demonstrates the effectiveness of surface-modified γ-Al2O3, which is reusable, efficient, catalytic, safe, and environmentally acceptable for the regioselective synthesis of 1,5-disubstituted-1,2,3-triazoles via [3 + 2] cycloaddition of phenyl and benzyl azides with a series of aryl nitroolefins in good yields. No adverse effect on substituents such as nitro, cyano, hydroxy, ether linkage, and halogens was observed. The catalyst could easily be recycled and was reused for nine runs without losing its activity.
- Nanjundaswamy, Hemmaragala M.,Abrahamse, Heidi
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supporting information
p. 967 - 974
(2015/03/30)
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- Application of reduced graphene oxide and carbon nanotube modified electrodes for measuring the enzymatic activity of alcohol dehydrogenase
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An electrochemical method was developed to measure the enzymatic activity of alcohol dehydrogenase (ADH) by monitoring the amount of reduced nicotinamide adenine dinucleotide (NADH) generated in the catalysed oxidation of ethanol by ADH. The concentration
- Wang, Xianlong,Li, Li,Wang, Yanping,Xu, Chongzheng,Zhao, Bo,Yang, Xiaodi
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p. 2195 - 2200
(2013/06/26)
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- High quality Al-doped ZnO thin films deposited using targets prepared by chemical coprecipitation
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In order to grow high-quality aluminum-doped zinc oxide films (AZO), the chemical coprecipitation method was adopted to synthesize ultra-fine AZO powder, in which Al2O3O was more easily and more uniformly doped in ZnO compared to the
- Cai,Jiang,Zhu,Wang
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p. 1461 - 1464
(2010/02/15)
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- An overview study of chlorination reactions applied to the primary extraction and recycling of metals and to the synthesis of new reagents
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Energy intensive classical metallurgical processes, the depletion of high-grade ores and primary sources push the scientific and technical communities to treat lean and complex ores as well as secondary metal resources for the recovery of valuable metals.
- Kanari,Allain,Joussemet,Mochón,Ruiz-Bustinza,Gaballah
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- The mechanochemical reduction of AgCl with metals : RRRRevisiting an experiment of M. Faraday
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Faraday induced the mechanochemical reduction of AgCl with Zn, Sn, Fe and Cu in 1820, using trituration in a mortar. This experiment is revisited, employing a mortar-and-pestle and a ball mill as mechanochemical reactors. The reaction kinetics depends both on the thermochemical properties and the hardness of the reactants. When using Zn as the reducing agent, Faraday likely observed a mechanically induced self-sustaining process (MSR), or at least he came very close to doing so.
- Takacs
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- Compositions of zirconium chloride complex and its method of manufacture
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The invention discloses a process for preparing highly active aluminum zirconium tetrochlorohydrate glycine powder by forming aluminum chloride glycine and zirconium chloride glycine solution individually, and then blending such aluminum chloride glycine and zirconium chloride glycine together to form aluminum zirconium tetrochlorohydrate glycine.
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(2010/11/24)
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- Sorption-active materials based on an acid-nonresistant aluminosilicate nepheline, used for defluorination of industrial sewage
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A method for obtaining sorption-active materials based on a solidifying mineral dispersion composed of nepheline, hydrochloric acid, and water was suggested. The hardening processes and conditions under which sorption-active compounds are formed were studied. The mechanism of sorption of F- ions on the sorbents developed was determined.
- Zosin,Priimak,Koshkina,Masloboev
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p. 1077 - 1083
(2008/02/04)
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- Electrochemical and spectroscopic studies of the chloro and oxochloro complex formation of Nb(V) and Ta(V) in NaCl-AlCl3 melts
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The equilibrium constant for the chloro complex formation of Nb(V) NbCl6-?NbCl5+Cl- (i) in NaCl-AlCl3 melts at 175°C was found to be pKi = 2.86(5). The oxochloro complex formation of Nb(V) and Ta(V) in NaCl-AlCl 3 melts at 175°C could be explained by the following equilibria: MOCl4-?MOCl3+Cl- (ii) MOCl 3?MOCl2++Cl- (iii) where M = Nb and Ta. The equilibrium constants determined by potentiometric measurements with chlorine-chloride electrodes were, for M = Nb, pKii, = 2.21(4) and pKiii = 3.95(5) and, for M = Ta, pKii = 2.743(15) and pKiii = 4.521(13). NbCl6- has two bands in the UV-vis region, a strong one at 34.7 × 103 cm-1 and a weaker one at 41.6 × 103 cm-1. The MOCl 4- complexes showed in the case of Nb(V) absorption bands at 32.7 and 42.9 × 103 cm-1 and in the case of Ta(V) at 38.6 and 48.1 × 103 cm-1.
- Von Barner,Bjerrum
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p. 9847 - 9851
(2008/10/09)
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- Power law behavior in chemical reactions
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Reactions between metals and chloride solutions have been shown to exhibit magnetic field fluctuations over a wide range of size and time scales. Power law behavior observed in these reactions is consistent with models said to exhibit self-organized criticality. Voltage fluctuations observed during the dissolution of magnesium and aluminum in copper chloride solution are qualitatively similar to the recorded magnetic signals. In this paper, distributions of voltage and magnetic peak sizes, noise spectra, and return times are compared for both reactions studied.
- Claycomb,Nawarathna,Vajrala,Miller
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p. 12428 - 12430
(2008/01/27)
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- Thermal and electrochemical C-X activation (X = Cl, Br, I) by the strong Lewis acid Pd3(dppm)3(Co)2+ cluster and its catalytic applications
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The stoichiometric and catalytic activations of alkyl halides and acid chlorides by the unsatured Pd3(dppm)3(CO)2+ cluster (Pd32+) are investigated in detail. A series of alkyl halides (R-X; R = t-Bu, Et, Pr, Bu, allyl; X = Cl, Br, I) react slowly with Pd32+ to form the corresponding Pd3(X)+ adduct and "R+". This activation can proceed much faster if it is electrochemically induced via the formation of the paramagnetic species Pd3+. The latter is the first confidently identified paramagnetic Pd cluster. The kinetic constants extracted from the evolution of the UV-vis spectra for the thermal activation, as well as the amount of electricity to bring the activation to completion for the electrochemically induced reactions, correlate the relative C-X bond strength and the steric factors. The highly reactive "R+" species has been trapped using phenol to afford the corresponding ether. On the other hand, the acid chlorides react rapidly with Pd32+ where no induction is necessary. The analysis of the cyclic voltammograms (CV) establishes that a dissociative mechanism operates (RCOCl → RCO+ + Cl-; R = t-Bu, Ph) prior to Cl- scavenging by the Pd32+ species. For the other acid chlorides (R = n-C6H13, Me2CH, Et, Me, Pr), a second associative process (Pd32+ + RCOCl → Pd32+Cl(CO)(R)) is seen. Addition of Cu(NCMe)4+ or Ag+ leads to the abstraction of Cl- from Pd3(Cl)+ to form Pd32+ and the insoluble MCl materials (M = Cu, Ag) allowing to regenerate the starting stating unsaturated cluster, where the precipitation of MX drives the reaction. By using a copper anode, the quasi-quantitative catalytic generation of the acylium ion ("RCO+") operates cleanly and rapidly. The trapping of "RCO+" with PF6- or BF4- leads to the corresponding acid fluorides and, with an alcohol (R′OH), to the corresponding ester catalytically, under mild conditions. Attempts were made to trap the key intermediates "Pd3(Cl)+...M+" (M+ = Cu+, Ag+), which was successfully performed for Pd3(ClAg)2+, as characterized by 31P NMR, IR, and FAB mass spectrometry. During the course of this investigation, the rare case of PF6- hydrolysis has been observed, where the product PF2O2- anion is observed in the complex Pd3(PF2O2)+, where the substrate is well-located inside the cavity formed by the dppm-Ph groups above the unsatured face of the Pd32+ center. This work shows that Pd32+ is a stronger Lewis acid in CH2Cl2 and THF than AlCl3, Ag+, Cu+, and Tl+.
- Lemaitre, Frederic,Lucas, Dominique,Groison, Katherine,Richard, Philippe,Mugnier, Yves,Harvey, Pierre D.
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p. 5511 - 5522
(2007/10/03)
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- Intermediates useful for the preparation of antihistaminic piperidine derivatives
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The present invention is related to a novel intermediates and processes which are useful in the preparation of certain antihistaminic piperidine derivatives of the formula whereinW represents —C(=O)— or —CH(OH)—;R1 represents hydrogen or hydroxy;R2 represents hydrogen;R1 and R2 taken together form a second bond between the carbon atoms bearing R1 and R2;n is an integer of from 1 to 5;m is an integer 0 or 1;R3 is —COOH or —COOalkyl wherein the alkyl moiety has from 1 to 6 carbon atoms and is straight or branched each of A is hydrogen or hydroxy; and pharmaceutically acceptable salts and individual optical isomers thereof,with the proviso that where R1 and R2 are taken together to form a second bond between the carbon atoms bearing R1 and R2 or where R1 represented hydroxy, m is an integer 0.
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- New representatives of the Er6[Si11N20]O structure type. High-temperature synthesis and single-crystal structure refinement of Ln(6+x/3)[Si(11-y)AlyN (20+x-y)]O(1-x+y) with Ln = Nd, Er, Yb, Dy and 0 ≤ x ≤ 3, 0 ≤ y ≤ 3
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According to the general formula Ln(6+x/3)-[Si(11-y)AlyN (20+x-y)]O(1-x+y) (0 ≤ x ≤ 3, 0 ≤ y ≤ 3) four nitridosilicates, namely Er6[Si11N20]O, Yb6.081[Si11N20.234]O0.757, Dy0.33Sm6[Si11N20]N, and Nd7[Si8Al3N20]O were synthesized in a radiofrequency furnace at temperatures between 1300 and 1650°C. The homeotypic crystal structures of all four compounds were determined by single-crystal X-ray diffraction. The nitridosilicates are trigonal with the following lattice constants: Er6[Si11N20]O: a = 978.8(4) pm, c = 1058.8(3) pm; Yb6.081[Si11N20.243]O0.757: a = 974.9(1) pm, c = 1055.7(2) pm; Dy0.33Sm6[Si11N20]N: a = 989.8(1) pm, c = 1078.7(1) pm; Nd7[Si8Al3N20]O: a = 1004.25(9) pm, c = 1095.03(12) pm. The crystal structures were solved and refined in the space group P31c with Z = 2. The compounds contain three-dimensional networks built up by corner sharing SiN4 and AlN4 tetrahedra, respectively. The Ln3+ and the isolated O2- ions are situated in the voids of the structures. According to Ln(6+x/3)[Si(11-y)AlyN (20+x-y)]O(1-x+y) an extension of the Er6[Si11N20]O structure type has been found. Wiley-VCH Verlag GmbH, 2001.
- Koellisch, Klaus,Hoeppe, Henning A.,Huppertz, Hubert,Orth, Michael,Schnick, Wolfgang
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p. 1371 - 1376
(2008/10/08)
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- Translucent antacid suspension
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An essentially translucent antacid composition is formed by an aqueous colloidal aluminum hydroxide gel wherein the average particle size of the aluminum hydroxide is less than about 0.5 microns, preferably less than about 0.1 microns, and more preferably less than about 0.01 microns. The suspension is further preferably mixed with a polyol, such as sorbitol or maltitol, to enhance the translucency. The weight ratio of polyol to aluminum hydroxide gel (USP) ranges from about 0.5:1.0 to about 4.0:1.0.
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- 1-arylsulphonyl, arylcarbonyl and arylthiocarbonyl pyridazino derivatives and methods of preparation
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1-Arylsulphonyl, arylcarbonyl and arylthiocarbonyl pyridazino derivatives and processes for making said derivatives are described. The novel derivatives are non-steroidal heterocyclic compounds which act as selective progestins and/or antiprogestins having a high in-vitro affinity for either the uterine, breast or bone progestin receptor. As such, the non-steroidal heterocyclic derivatives are useful in contraception, menopause, osteoporosis or endometriosis.
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- PROCESS FOR PREPARING 6-[(ISOXAZOLINYL)METHYL]PENICILLANIC ACID 1,1-DIOXIDE COMPOUNDS
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The invention provides a novel class of 6-(isoxazolinyl)methyl penicillanic acid 1,1-dioxide compounds having the formula: wherein M, X, R2, R3, R4 and R5 are described in the specification; which exhibit activity as a P-lactamase inhibitor.
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- Catalytic hydrogenolysis
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A process is disclosed for the catalytic hydrogenolysis of at least one starting material selected from saturated acyclic halofluorocarbons and hydrohalofluorocarbons containing three or four carbon atoms, and from one to five non-fluorine halogens (each non-fluorine halogen being independently chlorine or bromine) wherein all non-fluorine halogen substituents are contained on end carbons. The process involves reacting the starting material with hydrogen at an elevated temperature of about 300° C. or less in the presence of a catalyst containing a catalytically effective amount of palladium supported on carbon to produce a hydrogenolysis product wherein over 80 mole percent of the hydrogenolysis product is a saturated compound having the same distribution of fluorine substituents as the starting material. The carbon support has an ash content of less than about 0.5% by weight.
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- Process for producing polyhalogenated phthalocyanine
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A process for producing a polyhalogenated phthalocyanine containing not more than 0.02 part by weight of water-insoluble inorganic impurities derived from aluminum chloride per 100 parts by weight of phthalocyanine before halogenation, which comprises the following steps A, B and C; step A of halogenating phthalocyanine in titanium tetrachloride in the presence of aluminum chloride, step B of evaporating titanium tetrachloride and sublimating aluminum chloride by heating the halogenation reaction mixture, thereby recovering aluminum chloride as a mixture with titanium tetrachloride and obtaining a polyhalogenated phthalocyanine, and step C of recycling aluminum chloride isolated from the mixture with titanium tetrachloride or said mixture to the step A.
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- Polyhalogenated phthalocyanine, process for the production thereof, and use thereof
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A polyhalogenated phthalocyanine obtained by halogenation of phthalocyanine in the presence of aluminum chloride and contains not more than 0.02 part by weight, per 100 parts by weight of the phthalocyanine before the halogenation, of water-insoluble inorganic impurities derived from the aluminum chloride contributes to improvement of a printing ink in form plate abrasion properties.
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- Process for chlorofluoropropanes
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A process for the preparation of chlorofluoropropanes of the formula C3 HCl2 F5 by contacting monofluorodichloromethane with tetrafluoroethylene in the presence of a modified aluminum chloride catalyst at a temperature of 0° to 150° C. The novel compound CF3 CCl2 CHF2 is also disclosed.
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- Process for preparing fluorinated benzoyl compounds
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Fluorinated benzoyl compounds of the formula: STR1 wherein Q is a lower alkyl group, a halogen atom, --CH2 CO2 R1 wherein R1 is a lower alkyl group, or STR2 wherein each of R2 and R3 is a lower alkyl group, are disclosed.
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- Preparation of metal halide-amine complexes
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A process for the preparation of an amine complex of a metal halide which comprises reacting said metal with an amine hydrohalide. The process can be extended to the use of metals such as aluminum, magnesium, zinc, iron, and the like.
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- Gaseous Species in the Ti-Al-Cl System and Reaction with H2O
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Chemical species in the Ti-Al-Cl system at elevated temperatures were studied by effusion-beam mass spectrometry up to 1400 K.Gaseous TiAlCl5 and TiAlCl6 were identified as products of the reaction of TiCl4(g) and a Ti-Al mixture above about 900 K, for which AlCl3, TiCl2, and TiCl3 were also present.No evidence was found for TiAlCl7.When gaseous TiCl4, AlCl3, and H2O and admitted simultaneously, TiOCl2, Al(OH)Cl2, and TiAl(OH)Cl5 were observed.All ion species showed the correct isotopic distribution.The results confirm earlier indications that AlCl3 forms gaseous complexes with divalent and trivalent Ti, but not with tetravalent Ti.
- Hildenbrand, D. L.,Lau, K. H.
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p. 3435 - 3437
(2007/10/02)
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- Preparation of metal halide-amine complexes
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A process for the preparation of an amine complex of an aluminum trihalide which comprises reacting aluminum with an amine hydrohalide. The process can be extended to the use of other metals besides aluminum, e.g. magnesium, zinc, or iron.
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- Aluminum Dichloride and Dibromide. Preparation, Spectroscopic (Including Matrix Isolation) Study, Reactions, and Role (Together with Alkyl(aryl)aluminum Monohalides) in the Preparation of Organoaluminum Compounds
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Anhydrous aluminum trichloride or bromide when heated in a 2:1 molar ratio with aluminum powder as a suspension in dry n-heptane or methylcyclohexane was found to be partially reduced to aluminum dichloride or dibromide.Ultrasound treatment (sonication) significantly promotes the reaction.Aluminum dichloride in higher purity was obtained by the reaction of the gaseous aluminum trichloride with aluminum metal in a high-vacuum reactor, allowing subsequent investigation by IR spectroscopy.An aluminum sub-halide of the form Al2(i-Bu)4-xClx was also prepared through the reaction of the tetraisobutyldialane and HCl at room temperature.Both materials were investigated by IR spectroscopy and compared to AlCl2 prepared and isolated through the codeposition of aluminum atom and molecular chlorine in a solid argon matrix.The matrix study characterized AlCl2 together with AlCl and AlCl3, which were also formed in the system.The paramagnetic aluminum dihalides, i.e.AlCl2 and AlBr2, are associated in the condensed state (except under matrix isolation conditions where they are monomeric).An ESR study of the pyridinium complex of AlCl2 was carried out and showed its paramagnetic nature.In the present study, for simplicity, the reactions of the aluminum dihalide are considered as those of the dimers but could involve higher associated oligomers.MNDO calculation on the heats of formation of several possible isomeric structures of Al2Cl4 indicate the preference for both halogen bridging and significant Al-Al bonding in the dimer.Reaction of AlCl3 + Al with ethylene, the Hall and Nash reaction, was reinvestigated by 13C and 27Al NMR spectroscopy.The reaction was found to give, besides ethylaluminum sesquichloride, 1,2- and 1,1-bis(dichloroaluminio)ethanes.Cyclohexene in a similar reaction gives although less readily, 1,2-bis(dichloroaluminio)cyclohexane.The reaction are indicative of addition of (AlCl2)2 to the olefins.Aklyl- and arylaluminum monohalides are intermediately formed in the reaction of alkyl halides or halobenzenes with active aluminum powder.These divalent aluminum halides are also considered to be dimeric in nature and immediately react with excess of the alkyl (aryl) halides to form the corresponding sesquihalides.In contrast, aluminum dihalides formed in the aluminum trihalide-aluminum metal systems react with alkyl or aryl halides to give alkyl(aryl)aluminum dihalides.Sonication was found to significantly promote these reactions.
- Olah, George A.,Farooq, Omar,Farnia, S. Morteza F.,Bruce, Mark R.,Clouet, Francoise L.,et. al.
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p. 3231 - 3238
(2007/10/02)
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- Sinthesis and High-Pressure Behaviour of Quaternary Chalcogenide Halides M2M'X3Y (M = Zn, Cd; M' = Al, Ga, In; X = Se, Te; Y = Cl, Br, I)
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Quaternary chalcogenide halides M2M'X3Y (M = Zn, Cd; M' = Al, Ga, In; X = Se, Te; Y = Cl, Br, I) can be synthesized by heating stoichiometric amounts of the binary components MX, MY2, and M'2X3 in evacuated sealed quartz ampoules.In the case of aluminium and gallium compounds, a mixture of the M' and X elements rather than the binary compounds has been used.The products are typical tetrahedral compounds, crystallizing with either the defect wurtzite-type or the defect zinc-blende-type structure.At 25 kbar, and 1400 deg C, Cd2InSe3Cl, Cd2InSe3Br, and Cd2InSe3I transform from the defect wurtzite-type structure to quenchable high-pressure phases with defect NaCl-type structure.The retransformation to the ambient-pressure phases proceeds via intermediates having the defect zinc-blende-type structure.Some aspects of the apparent nonstoichiometry in the high-pressure phases are discussed. - Keywords: Quaternary Chalcogenide Halides, Synthesis, Crystal Structure, High-Pressure Reactions
- Range, Klaus-Juergen,Handrick, Karin
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p. 153 - 158
(2007/10/02)
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- Pentaerythritol derivative
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Complexes of pentaerythritol derivatives such as sulfuric acid ester of pentaerythritol or dipentaerythritol with a basic polyaluminum chloride and process for preparing the same are disclosed. The complex is novel and has a good anti-pepsin activity and therefore it is useful as an anti-ulcer agent.The complex is prepared by reacting pentaerythritol or dipentaerythritol with a sulfating agent and then reacting the resulting sulfate with a basic polyaluminum chloride.
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- Vasodilator compound and pharmaceutical compositions therefrom
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The compound N-(2,6-dichlorophenyl)acetamidine STR1 and its addition salts with pharmaceutically compatible inorganic and organic acids, exhibit a fast, strong vasodilator and antihypertensive action, which is of prolonged duration.
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- NbAlCl8: A molecular dinuclear complex in the solid, melt, and vapor phases. Synthesis, crystal structure, and raman spectra
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Crystalline NbAlCl8 was prepared as a new type of dinuclear halide complex by the direct reaction of Al2Cl6 with Nb2Cl10 at ～200°C in evacuated sealed glass ampoules. The yellow compound is orthorhombic, space group Cmcm, with a = 8.016 (2) A?, b = 17.139 (4) A?, c = 8.116 (2) A?, V = 1115.1 A?3, Dmeasd = 2.40 (2) g·cm-3, and Dcalcd = 2.403 g·cm-3 for Z = 4. The crystal and molecular structure determination was based on three-dimensional X-ray diffractometer data refined to a final conventional R factor of 0.030 for 639 independent reflections with I ≥ 2σ(I). The crystals contain dinuclear Cl4NbCl2AlCl2 molecules with mm symmetry, consisting of an AlCl4 tetrahedron sharing a common edge with a distorted NbCl6 octahedron. Al-Cl bond lengths of 2.078 (2) and 2.200 (2) A? and Nb-Cl bond lengths of 2.219 (1), 2.288 (1), and 2.643 (1) A? were observed. The Nb-Cl bridge bonds are longer than in the Nb2Cl10 molecule, thus indicating a higher Lewis acidity of AlCl3 compared to that of NbCl5. Polarized Raman spectra of NbAlCl8 single crystals were obtained at room temperature. The factor-group analysis of vibrations in crystalline NbAlCl8 was used for the assignment of the observed Raman bands. Raman spectra of melt mixtures of NbCl5 with AlCl3 at 235°C were characterized by a superposition of bands due to Al2Cl6(l), Nb2Cl10(l), and NbCl5(l), together with NbAlCl8(1). Measurements of relative Raman band intensities in the mixtures showed two strongly polarized bands at 416 and 364 cm-1 and other weaker bands due to NbAlCl8 complexes present in the melts. Raman spectra of vapors over the liquid mixtures at temperatures between 235 and 350 °C were mainly due to Al2Cl6(g) and NbCl5(g) molecules. Two new polarized bands observed in the spectra at 418 and 369 cm-1 were attributed to the formation of the NbAlCl8 gaseous molecule.
- Krebs, Bernt,Janssen, Holger,Bjerrum, Niels J.,Berg, Rolf W.,Papatheodorou
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p. 164 - 171
(2008/10/08)
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- Gaseous complexes of nickel chloride with aluminum chloride and gallium chloride
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The thermodynamic functions ΔH and ΔS of the reactions (A) NiCl2(s) + LCl3(g) = NiLCl5(g) and (B) NiCl2(s) + L2Cl6(g) = NiL2Cl8(g) (L = Al, Ga) have been determined by spectrophotometry of the gas phase from 300 to 840°C and by quenching of the equilibrated gas phase and analysis of the condensates. From combination of the results with a previous study where L = In it is found that ΔS does not depend significantly on L but is approximately 70 J mol-1 K-1 for reaction A and approximately 43 J mol-1 K-1 for reaction B. For reaction A ΔH is most positive for L = Ga, making the Ga complexes the least stable ones of the series where L = Al, Ga, In. This stability sequence follows the dimerization energies of LCl3. The observed trend of the thermodynamic functions and the similarity of the spectra suggest that the structures of all NiLCl5 complexes on one hand and of all the NiL2Cl8 complexes on the other hand are similar.
- Emmenegger,Favre,Kluczkowski
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p. 2934 - 2938
(2008/10/08)
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- Preparation of chromane derivatives
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Chromane derivatives (I) STR1 where R1, R2 and R3 are H or C1 -C8 -alkyl, R4 is H, C1 -C8 -alkyl or C1 -C8 -acyl and R5 is C1 -C8 -alkyl are prepared by reacting a hydroquinone (II) STR2 with a Lewis acid or a Lewis acid derivative having the same action, and with a nitrile CH2 =CH--C(R5)(OR6)CN (III), where R6 is H, C1 -C4 -acyl or C1 -C4 -alkyl, or with a compound from which III is formed in situ, in the presence of an inert solvent.
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- Reaction between Aluminium Trichloride and Oxygen in the Vapor Phase and Properties of the Aluminium Oxide Formed
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The reaction between gaseous AlCl3 and oxygen occurs at above ca. 400 deg C and proceeds appreciably above ca. 800 deg C to form Al2O3 and chlorine.The Al2O3 formed is amorphous Al2O3 at 800 deg C, γ-Al2O3 containing amorphous Al2O3 at 900 and 950 deg C,
- Shoji, Yuichi,Tatsumii, Kimikazu,Matsuzaki, Ryoko,Saeki, Yuzo
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p. 269 - 270
(2007/10/02)
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- Certain pharmaceutical sulfamoylbenzoyl benzofurans, benzothiophenes, and indoles
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Heterocyclic sulfamoyl-aryl-ketones wherein the heterocyclic component consists of a benzofuran, indole or benzothiophene radical and the sulfamoyl-aryl moiety is ortho-substituted by halogen, methyl or trifluoromethyl having uricosuric, hypouricemic and salidiuretic action and a process for their manufacture.
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- Aluminum catalysts
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An aluminum halide complex of an aluminum halide, a hydrogen halide and an alkylbenzene is prepared by continuously feeding a gaseous hydrogen halide to a reaction zone comprising aluminum and an alkylbenzene and continuously taking the resulting aluminum halide complex out of the reaction zone, the byproduced hydrogen gas being taken out of the reaction zone, and aluminum and the alkylbenzene being fed continuously or intermittently to the reaction zone.
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