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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
Authors:V.V. Shatunov  A.A. Korlyukov  A.V. Lebedev  B.I. Kozyrkin  V.Yu. Orlov
Affiliation:a State Scientific Center RF GNIIChTEOS, 38, shosse Entuziastov, Moscow 111123, Russia
b A.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Vavilova str. 28, 119991, Moscow, Russia
c JSC Alkyl, d. 3, str. 1, proezd 4807, Zelenograd, Moscow, 124489, Russia
Abstract: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.
Keywords:Gallium trialkyls   Aluminum trialkyls   Indium trialkyls   Triphenylphosphine   Bis(diphenylphosphine)alkanes   Synthesis
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