17150-84-4Relevant articles and documents
Preparation of organogallium compounds from organolithium reagents and gallium chloride. Infrared, magnetic resonance, and mass spectral studies of alkylgallium compounds
Kovar, Roger A.,Derr, Henry,Brandau, Duane,Callaway, John Owen
, p. 2809 - 2814 (2007/10/06)
Conditions for the preparation of a series of base-free trialkylgallium compounds in benzene solvent by the exchange reaction of alkyllithium compounds and gallium chloride are described. Optimum conditions which favor formation of the trialkyl involve mixing a benzene solution of an appropriate alkyllithium compound and a benzene solution of gallium chloride in exactly a 3:1 molar ratio, heating of the reaction mixture for 12 hr at 70°, filtration to remove by-product lithium chloride, removal of solvent under vacuum, and vacuum distillation of the product: 3RLi + GaCl3 = 3LiCl + R3Ga, where R = C2H5, n-C3H7, n-C4H9, i-C4H9, s-C4H9, and t-C4H9. Alkylgallium dichlorides and dialkylgallium chlorides are produced when lithium alkyls and gallium chloride are allowed to react in a 1:1 and 2:1 molar ratio, respectively: nRLi + GaCl3 = nLiCl + RnGaCl3-n, where n = 1 and 2. Reaction of an alkyllithium compound and gallium chloride in a molar ratio in excess of 3:1 results in formation of the corresponding lithium tetraalkylgallate: 4n-C3H7Li + GaCl3 = 3LiCl + LiGa(n-C3H7)4. Trivinylgallium tetrahydrofuranate is produced by the reaction of vinyllithium and gallium chloride in 3:1 molar ratio in tetrahydrofuran solvent. Infrared, proton magnetic resonance, and mass spectra of RnGaCl3-n compounds where R = C2H5 to C4H9 isomers and n = 1-3 are reported and discussed. Proton magnetic resonance spectra reveal that the chemical shifts for protons on α-carbon atoms are sensitive to substitution on the gallium. An explanation for these chemical shift data along with molecular association data for RnGaCl3-n. compounds is given. Mass spectroscopy can be used as a convenient, diagnostic tool for the identification of organogallium compounds of this type. Ion abundance data for all compounds are presented and the fragmentation processes believed to give these ions are discussed.
