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, D; CALLAWAY, JOHN OWEN

doi:10.1021/ic50153a042

Cited by 103 publications

(41 citation statements)

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“…Precursor Preparation: The precursors (tBu) 3 Ga and As(SiMe 3 ) 3 were prepared by literature methods [16,17]. GaCl 3 was purchased and used as received from STREM.…”

Section: Methodsmentioning

confidence: 99%

Supercritical Fluid–Liquid–Solid Synthesis of Gallium Arsenide Nanowires Seeded by Alkanethiol‐Stabilized Gold Nanocrystals

et al. 2004

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The impetus for new methods in nanomaterials chemistry derives from the need for effective and tunable routes to nanostructures with any desired composition, structure, shape, size, and interfacial properties. Nanowires represent an important class of materials, having the characteristics of one-dimensional quantum confinement when smaller than a critical diameter and the potential to electrically connect the components in an integrated nanoscale system. Several general synthetic strategies for nanowires have been developed, including vapor-phase and solution-phase routes.[1] Many different semiconductor materials have been produced using vaporphase routes by the vapor±liquid±solid (VLS) growth mechanism, [1±3] a process that relies on a metal particle to seed and direct semiconductor wire formation. In solution, a variety of nanowire materials have been synthesized without growth catalysts, however the unidirectional morphology of these nanostructures primarily reflects an internal anisotropic crystal structure.[1] Therefore, researchers (including us) have sought to combine VLS growth with solution-phase chemistry to develop a general route to nanowire synthesis that does not depend on crystal structure. [4,5] The challenge of combining VLS with solution-phase chemistry is the required synthetic temperatures that must exceed the seed metal/semiconductor eutectic temperature. In their pioneering work, Buhro and co-workers demonstrated VLStype nanowire synthesis in conventional solvents (called solution±liquid±solid (SLS)) at synthetic temperatures of around 200 C, using metal/semiconductor combinations such as Ga/ GaAs, [4] In/InN, [6] and, most recently, In/GaAs [7] with low eutectic temperatures. Unfortunately, the eutectic temperatures for most metal/semiconductor combinations are greater than 350 C, including the group IV semiconductors, Si and Ge (with Au). These reaction temperatures can be accessed in solution by pressurizing the solvent above its critical point.Recently, we demonstrated Si and Ge nanowire synthesis in supercritical hexane at temperatures ranging from 350 C to 500 C and pressures ranging from 100 atm to 370 atmÐa process we have called supercritical fluid±liquid±solid (SFLS) nanowire growth. [5,8±10] Hypothetically, this process could be applied to any semiconductor/metal combination with eutectic temperatures less than 600 C Ðthe maximum temperature before degradation of most organic solvents. Here, we demonstrate the first SFLS nanowire synthesis of a compound semiconductor material: GaAs. GaAs nanowires were synthesized in supercritical hexane at 500 C and 37 MPa (370 atm) by reacting (tBu) 3 Ga and As-(SiMe 3 ) 3 in the presence of dodecanethiol-stabilized 7 nm Au nanocrystal seeds. High yields of nanowires (60 %) could be obtained with very little particulate formationÐthe GaAs nanowires shown in Figure 1a were taken directly from the reactor without any purification. They were synthesized with 10 mM precursor solution concentration with a 100:1 precursor/gold molar ratio. These pr...

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“…Precursor Preparation: The precursors (tBu) 3 Ga and As(SiMe 3 ) 3 were prepared by literature methods [16,17]. GaCl 3 was purchased and used as received from STREM.…”

Section: Methodsmentioning

confidence: 99%

Supercritical Fluid–Liquid–Solid Synthesis of Gallium Arsenide Nanowires Seeded by Alkanethiol‐Stabilized Gold Nanocrystals

et al. 2004

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“…NMR spectra were recorded in C 6 [47] (synthesised from EtLi and GaCl 3 ), was isolated in high yield from the reaction of commercially available ZnEt 2 (Sigma Aldrich) and GaCl 3 (see below). Et 2 AlH and iBu 2 Al-H were purchased from MOCHEM GmbH, Marburg, Germany, and used without further purification.…”

Section: Methodsmentioning

confidence: 99%

Hydroalumination versus Deprotonation of Alkynes with Sterically Demanding Substituents

Uhl

Layh

Rhotert

et al. 2013

Zeitschrift Für Naturforschung B

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Treatment of sterically highly shielded terminal alkynes, H-C≡C-aryl, with dialkylaluminium and dialkylgallium hydrides, R 2 E-H, afforded by hydrogen release dimeric dialkylelement alkynides with a four-membered E 2 C 2 heterocycle independent of the bulk of the aryl groups. A rare example of a monomeric alkynylaluminium compound was only obtained with very bulky CH(SiMe 3 ) 2 groups attached to the metal atoms and by salt elimination reaction. The steric shielding by the bulky aryl groups did not prevent condensation reactions. Hydroalumination of 1-(trimethylsilyl)-2-(2,6-dimethylphenyl)ethyne using Me 2 Al-H resulted in a divinyl compound by elimination of trimethylaluminium.

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“…Electron impact mass spectra were analysed using a Varian mass spectrometer. HGaCl 2 , [13] EtLi, [33] PhÀ CC-SiPh 3 (1 a), [34] PhC(H)=CA C H T U N G T R E N N U N G (SiPh 3 )GaCl 2 (2 a) [12] …”

Section: Methodsmentioning

confidence: 99%

“…The solution structures of the above compounds in the presence of polar solvents (Et 2 O, THF, tetramethylethylenediamine (TMEDA)) have been studied in detail by multinuclear one-and two-dimensional NMR spectroscopy on 6 Li-enriched samples. According to these studies, (nBu)C 6 H 4 (Li)C=C(Li)PhA C H T U N G T R E N N U N G (TMEDA) 2 [33] was found to be monomeric in solution and the solid state, whereas solutions of both compounds in Et 2 O or THF in the absence of TMEDA led to dimeric heterocubane-type structures or a mixture of monomers and dimers, respectively. [31,32] Compound 6 has a unique molecular structure (Figure 4a) with nine lithium atoms that are arranged in such a way as to generate two octahedra (Figure 4c) that share a common face (Li3, Li4, Li4').…”

Section: Wwwchemeurjorgmentioning

confidence: 99%

Vinylgallium and Alkyllithium Compounds: Transmetalation and Generation of Oligolithium Cages

Uhl

Kovert

Layh

et al. 2011

Chemistry A European J

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Vinylgallium compounds [C(6)H(6-n){(H)C=C(SiR(2) R')-GaR''(2)}(n ] (3, R=Ph, Me; R'=Ph, Me; R''=tBu, Et; n=1, 2) are easily accessible by hydrogallation of the corresponding alkynylbenzene derivatives with H-GaCl(2) and subsequent reaction with alkyllithium derivatives. Treatment of 3 with an excess amount of tert-butyl- or ethyllithium yielded by transmetalation and ortho-deprotonation of the aromatic rings the unprecedented solvent-free oligolithium cluster compounds [{(C(6)H(4)Li)HC=C(SiPh(3))Li}(2)(tBuLi)(2)] (4), [{(C(6)H(4)Li)HC=C(SiPh(2)Me)Li}(4)] (5) and [{(C(6)H(3)Li){HC=C(SiMe(3))Li}(2)}(3)] (6) in moderate yields. Their solid-state structures revealed the presence of unique molecular lithium clusters with 6, 8, or 9 lithium atoms that may be derived from two edge-sharing Li(4) tetrahedra (4), three Li(4) tetrahedra in a chain joined by two common edges (5) or a tricapped trigonal prism of lithium atoms (6).

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Preparation of organogallium compounds from organolithium reagents and gallium chloride. Infrared, magnetic resonance, and mass spectral studies of alkylgallium compounds

Cited by 103 publications

References 1 publication

Supercritical Fluid–Liquid–Solid Synthesis of Gallium Arsenide Nanowires Seeded by Alkanethiol‐Stabilized Gold Nanocrystals

Supercritical Fluid–Liquid–Solid Synthesis of Gallium Arsenide Nanowires Seeded by Alkanethiol‐Stabilized Gold Nanocrystals

Hydroalumination versus Deprotonation of Alkynes with Sterically Demanding Substituents

Vinylgallium and Alkyllithium Compounds: Transmetalation and Generation of Oligolithium Cages

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