- Synthesis of Heterobimetallic Group 13 Compounds via Oxidative Addition Reaction of Gallanediyl LGa and InEt3
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Equimolar amounts of LGa (L = [(2,6-i-Pr2-C6H3)NC(Me)]2CH) and InEt3 were found to react with insertion into the In-carbon bond and formation of LGa(Et)InEt2 (1), while in the presence of the N-heterocyclic carbene It-Bu [C(Nt-Bu2CH)2], the base-stabilized compound LGa(Et)Et2In←It-Bu (2) was formed, which shows an abnormal binding mode of the NHC group. In addition, the reaction of InEt3 with two equivalents of LGa occurred with double insertion and formation of [LGa(Et)]2InEt (3). 1-3 were characterized by heteronuclear NMR (1H, 13C) and IR spectroscopy, their solid-state structures were determined by single-crystal X-ray analyses, and their thermal stability was investigated by in situ NMR spectroscopy. (Chemical Equation Presented).
- Ganesamoorthy, Chelladurai,Bl?ser, Dieter,W?lper, Christoph,Schulz, Stephan
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p. 2991 - 2996
(2015/06/30)
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- Zirconium-catalyzed reaction of terminal alkenes with triethylindium
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Terminal alkenes (undec-1-ene, oct-1-ene, and allylbenzene) reacted with triethylindium in the presence of a catalytic amount of Cp2ZrCl 2 in hexane to give mixtures of three organoindium compounds whose hydrolysis in D2O afforded 2-substituted 1,4-dideuterobutane containing minor amounts of 2-substituted 1- and 4-deuterobutanes.
- Ramazanov,Dil'Mukhametova,Dzhemilev
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p. 1253 - 1256
(2013/11/06)
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- The synthesis and deep purification of GaEt3. Reversible complexation of adducts MAlk3 (M = Al, Ga, In; Alk = Me, Et) with phenylphosphines
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Optimal parameters of organomagnesium technique of synthesis of triethylgallium have been defined. Various techniques of deep purification of triethylgallium to the extent required in metalorganic vapor-phase epitaxy MOVPE have been studied: by way of residue ether displacement through high-performance rectification and interaction with high pure aluminum and gallium trichloride, and by way of reversible complexation with triphenylphosphine, 1,3-bis(diphenylphosphine)propane and 1,5- bis(diphenylphosphine)pentane. Advantages and disadvantages of each technique have been identified. We have shown high performance of adduct purification technique covering trimethyl and triethyl derivatives of aluminum, gallium and indium. The structure of donor-acceptor complexes between metal alkyls and the above-mentioned phosphines have been verified using H and 31P NMR spectroscopy and X-ray studies, as well as quantum chemical calculations. Thermal stability of triethylgallium and oxidation of its adducts with phosphines have been studied.
- Shatunov,Korlyukov,Lebedev,Sheludyakov,Kozyrkin,Orlov, V.Yu.
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p. 2238 - 2251
(2011/06/22)
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- Preparation of organometal compounds
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A method of preparing organometal compounds that does not use oxygenated solvents is provided. The compounds produced by such method are particularly useful as precursor compounds for metalorganic chemical vapor deposition processes used in the manufacture of electronic devices. Methods of depositing metal films using such organometal compounds are also provided.
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- Synthesis, mass spectrometry and nmr spectroscopy studies of the (ch3) 2in(c2h5) system: X-ray crystal structure of a diphosphine-bridged complex
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The synthesis of homoleptic and heteroleptic alkylindium derivatives (generally as diethyl ether adducts) was carried out in high yields from InI3. The nuclear magnetic resonance and mass spectra of the compounds MenInEt3n (n = 0, 1, 2, or 3) and of their trideuteromethyl analogues showed that both heteroleptic Me2InEt and MeInEt2 exist as single compounds, although disproportionation to InMe3 and InEt3 has been observed at temperatures slightly higher than room temperature. The crystal structure of unusual diphosphine-bridged adduct, [(InMe3)diphos(Me2InEt)] · [(InMe3)diphos(InMe3)], (diphos = (C6H5)2PCH2CH2P(C6H5)2 is reported.
- Visona,Benetollo,Rossetto,Zanella,Traldi
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- Purification of tri-alkyl compounds of Group 3a metals
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A tri-alkyl compound of a Group 3a metal is purified by a process in which a polyether of the formula STR1 wherein R independently is alkyl of 1 to 4 carbon atoms inclusive, each R' independently is hydrogen, methyl or ethyl; m is an integer from 1 to 6 inclusive; and n is an integer from 1 to 12 inclusive, is added to a composition comprising a tri-alkyl compound and the polyether. The adduct is heated to dissociate the adduct thermally into a mixture containing tri-alkyl compound of the Group 3a metal, and the mixture is subjected to distillation to recover the tri-alkyl compound of the Group 3a metal.
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