- Oxidation of metallic copper with complexones in organic media
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Direct oxidation of copper in organic media with complexones (sterically hindered o-quinones; acetylacetone and pyridine as stabilizing ligands) was studied. From the complexes obtained, the initial components can be regenerated.
- Klimov,Davydova,Buzaeva,Dubrovina,Kalyukova
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- Synthesis, structure and reactivity of schiff base transition metal mixed ligand complexes derived from isatin and salal
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A series of Isatin derivative Schiff base ligands have been prepared by the nucleophilic addition of 5-Bromo isatin with various amine derivatives and characterized by CHNS analysis and spectral data. Similarly, two of salicylaldehyde ligand have been prepared by the nucleophilic addition of Salal with amine derivatives. In order to investigate the coordination behavior of these ligands and their metal complexes of the type M(acac)x, L [M = Cu(II), Ni(II); L = Schiff base ligands; x = 0 or 2] mixed ligand (chelate) have been prepared from the reaction of these ligands with their corresponding metal (Ni, Cu) acetylacetonates. The present paper was an approach to understand the chelating mixed ligand formation in complexes. All the isolated Shiff base ligands and mixed acac metal complexes were characterized by using IR, 1H NMR, UV-Vis, molar conductance and TGA/DTA analysis. The biological activities of all the isolated ligands and their corresponding mixed acac metal complexes have been used to screening against the microorganisms both Gram-positive and Gram-negative bacteria such as E.coli and S.sureus respectively, fungi A. niger and C.albicans and the results have been compared with standard and control. The main idea of these types of biological screening is to understand the role of these isolated compounds in pharmaceutical industries for drug development.
- Sridevis,Girija,Satish
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p. 169 - 176
(2021/03/29)
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- Copper acetylacetonate and preparation method thereof
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The invention relates to the technical field of chemical product production, in particular to copper acetylacetonate and a preparation method thereof. A prepared high-activity copper salt and acetylacetone are subjected to a chemical reaction in a liquid phase formed by an organic solvent, the high-activity copper salt and acetylacetone are in full contact through an ultrasonic oscillation method,the contact area of the high-activity copper salt and acetylacetone is increased, the reaction probability of the high-activity copper salt and acetylacetone is increased, and therefore the yield andpreparation efficiency of copper acetylacetonate are effectively improved; furthermore, a washing and suction filtration treatment method is adopted in the process of preparing the copper salt raw material, a column chromatography separation method is adopted in the process of preparing the high-activity copper salt, and recrystallization and suction filtration methods are matched for use in theprocess of preparing the copper acetylacetonate, so that the prepared copper acetylacetonate is less in impurities, and the purity of the copper acetylacetonate is improved. The purity is further improved; the prepared copper acetylacetonate can be used as an organic synthesis catalyst, a resin cross-linking agent, a curing accelerator, a rubber additive and a fuel oil additive.
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Paragraph 0020-0051
(2021/01/15)
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- Reaction of the framework 3d-organometallosiloxanes with acetylacetone
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A reaction of acetylacetone with the framework sandwich-type metallosiloxanes (MOS) of general formula [PhSiO2]6M 6[PhSiO2]6, where M = Cu, Ni, Mn, was studied by GPC, 1H and 29Si NMR spectroscopy, X-ray diffraction, elemental and functional analysis. The reaction involved replacement of the metal atoms with the hydrogen atoms and is accompanied by the formation of the corresponding chelate complexes M(acac)2. Displacement of the metal from the framework MOS leads to the destruction of molecular skeleton and formation of phenylsiloxanes containing Si-OH groups. The yield and composition of the reaction products considerably depend on the nature of the metal in [PhSiO2]6M6[ThSiO2]6. A selective substitution of the metal leads to the stereoregular hexahydroxyhexaphenylcyclohexasiloxane, [PhSiO(PH)]6, cis-isomer. The structure and composition of the crystalline hexahydroxyhexaphenylcyclohexasiloxane obtained were confirmed by 29Si NMR spectroscopy, X-ray diffraction study, and functional analysis, while its TMS derivative was studied with 1H NMR spectroscopy and GPC. Using a framework manganese phenylsiloxane as an example, a reversible character of the process has been established and an alternative synthesis of this compound from hexahydroxyhexaphenylcyclohexasiloxane and Mn(acac)2 has been accomplished for the first time.
- Sergienko,Cherkun,Myakushev,Korlyukov,Zavin
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p. 1369 - 1375
(2011/04/16)
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- Influence of the counter anion and solvent in the structure of copper derivatives with the 2,3-bis(2-pyridyl)pyrazine ligand
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Several compounds have been isolated from the reaction between different copper bis(acetylacetonato) derivatives and the potentially bridging ligand 2,3-bis(2-pyridyl)pyrazine (bppz). A compound of formula [Cu(tfacac) 2(bppz)] (1) is obtained when the substituted trifluoromethylacetylacetonato is used. The use of different anions and the unsubstituted acetylacetonato give rise to new derivatives of general formula [{Cu(acac))2(μ-bppz)2]X2 (X-- BF4-, 2; PF6-, 3; BPh 4-, 4). In these compounds the bppz ligand is acting as a bridge by chelating one copper atom and bonding monodentate a second copper atom. The presence of anions with different coordination abilities introduces variations in the copper environment and geometry. When the non-coordinating tetraphenylborate is used different compounds depending on the nature of the solvent are obtained. The dimer 4 was isolated from a methanol/chloroform mixture, while in the absence of chloroform the monomeric compound of formula [Cu(acac)(bppz)(ROH)](BPh4)-ROH (ROH=MeOH, 5) was obtained. When ethanol was used instead of methanol the analogous derivative 6 (R=EtOH) was isolated. Both species show a mononuclear structure with the copper atom five-coordinated by the chelating acac and bppz ligands and one hydroxo group occupying the apical position. A similar environment for the copper appears in [Cu(tfacac)(bppz)(MeOH)](BPh4), 7, which shows a dimeric structure through hydrogen bonds interactions. The magnetic susceptibility data of the dimeric compounds show very weak antiferromagnetic interactions between the copper atoms, an expected fact since the bridging bppz ligand is not planar but the monodentate pyridine is more or less perpendicular to the other two aromatic rings, precluding the spin exchange via the it ligand electrons.
- Gutiérrez, Angel,Felisa Perpi?án,Sánchez, Ana E.,Carmen Torralba,Rosario Torres,Pilar Pardo
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p. 2443 - 2451
(2011/02/16)
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- PROCESS FOR THE PREPARATION OF METAL ACETYLACETONATES
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The present invention provides an improved, economical and environmmentally benign process for metal complexes of acetylacetone having the general formula, M(acac)n wherein M is a metal cation selected from the group consisting of Fe, Co, Ni, Cu, Zn, Al, Ca, Mg, Mo, Ru, Re, U, Th, Ce, Na, K, Rb, Cs, V, Cr, and Mn etc., n is an integer which corresponds to the electrovalence of M, are obtained by reacting the corresponding metal hydroxide, metal hydrated oxide or metal oxide with a stoichiometric amount of acetylacetone and separating the product.
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- Copper(II) complex with acetylacetone phenylhydrazone: Synthesis, crystal structure, and thermal stability
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The Cu(phac)2 complex was synthesized by the reaction of copper(II) acetate with acetylacetone phenylhydrazone (Hphac), and its crystal structure was established by X-ray diffraction: space group P21/c, a = 11.173(3) ?, b = 8.267(2) ?, c = 12.633(4) ?, β = 115.01(3)°, V = 1057.5(5) ?3, Z = 4, R1 = 0.0476. The crystal structure of Cu(phac)2 consists of the centrosymmetrical mononuclear molecules. The central copper(II) ion is coordinated by two oxygen atoms and two nitrogen atoms of two acetylacetone phenylhydrazone ligands. The Cu(phac)2 molecules are linked in layers parallel to the Oyz plane. The oxygen atoms of the ketone fragment are involved in intermolecular bonding, which completes the coordination sphere of the central copper(II) ion to a substantially elongated octahedron. The thermal stability of the Cu(phac)2 complex was estimated under nitrogen at atmospheric pressure and in vacuo.
- Kuz'mina,Eliseeva,Balashov,Troyanov
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p. 1182 - 1186
(2008/10/08)
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- Chemistry of copper(I) β-diketonate complexes. 2. Synthesis, characterization, and physical properties of (β-diketonato)copper(I) trimethylphosphine and bis(trimethylphosphine) complexes
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The volatile copper(I) complexes (β-diketonate)Cu(PMe3)n where β-diketonate = hexafluoroacetylacetonate (hfac), trifluoroacetylacetonate (tfac), and acetylacetonate (acac) for n = 1 and 2 and β-diketonate = dipivaloylmethanate (dpm) and dibenzoylmethanate (dbm) for n = 1 have been prepared in high yield. These species have been characterized by spectroscopy and by elemental analysis. A number of derivatives have been characterized by single-crystal X-ray diffraction. The compound (hfac)Cu(PMe3) crystallizes in the space group P1 with α = 10.801 (2) A?, b = 12.676 (3) A?, c = 14.946 (3) A?, α = 91.10 (3)°, β = 100.65 (3)°, γ = 94.06 (3)°, Z = 6, R = 6.71%, and Rw = 7.26% for 3751 reflections. The compound (dpm)Cu(PMe3) crystallizes in the space group P1 with a = 10.193 (3) A?, b = 12.059 (3) A?, c = 14.547 (3) A?, α = 96.40 (2)°, β = 91.54 (2)°, γ = 90.65 (2)°, Z = 4, R = 5.34%, and Rw = 5.57% for 5261 reflections. The compound (dbm)Cu(PMe3) crystallizes in the space group Cmc21 with a = 18.776 (6) A?, b = 7.995 (3) A?, c = 11,872 (4) A?, Z = 4, R = 2.72%, and Rw = 2.83% for 1620 reflections. While (acac)Cu(PMe3) and (tfac)Cu(PMe3) have only limited thermal stability, (hfac)Cu(PMe3) is thermally stable for at least 4 days at its melting point (67°C). The vapor pressure of (hfac)Cu(PMe3) has been measured as a function of temperature, revealing reasonable volatility (100 mTorr at 60°C). From the plot of log (vapor pressure) versus reciprocal temperature, an enthalpy of vaporization (ΔHvap) of approximately 10 kcal/mol was obtained.
- Shin,Chi,Farkas,Hampden-Smith,Kodas,Duesler
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p. 424 - 431
(2008/10/08)
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