Multinuclear NMR studies of the reactions of (Me3Al)2 with Me2AsNMe2, MeAs(NMe2)2 and As(NMe2)3

Krannich, L. K.; Watkins, Charles L.; Srivastava, D. K.

doi:10.1016/s0277-5387(00)80582-3

Cited by 17 publications

(5 citation statements)

References 53 publications

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“…The 13 C and 1 H NMR data, listed in the Experimental Section, are comparable to those reported for the corresponding methylaluminum derivatives, [Me 2 AlR] 2 . , The EI-MS data for the compounds confirmed their dimeric nature by giving masses for the appropriate dimer minus an isobutyl group (M + − Bu i ). Al−N compounds of this type typically give mass peaks that result from cleavage of an alkyl ligand off the aluminum atom. ,− , The IR data show no peaks in the range 3200−3300 cm -1 (indicative of N−H stretches derived from adducted secondary amines) 13 nor in the range 1700−1850 cm -1 (derived from Al−H stretches)…”

Section: Resultssupporting

confidence: 65%

“…Herein we report an NMR investigation on the reactivity of a series of monoaminodimethylarsines, Me 2 AsR [R = NMe 2 , NPr n 2 , NPr i 2 , NBu n 2 , NBu i 2 , NC 4 H 8 , NC 5 H 10 , NC 6 H 12 , and N(C 2 H 4 ) 2 NMe], toward Me 2 AlH and Bu i 2 AlH and note the influence that a variation in the steric bulk of R and the aluminum alkyl moiety has on overall reactivity and aminoalane dimer formation. For the Me 2 AlH/Me 2 AsR system, the resultant [Me 2 AlR] 2 products are compared with previously characterized samples from the reactions of Me 3 Al with the same aminoarsine series. , Because only [Bu i 2 AlNMe 2 ] 2 and [Bu i 2 AlNC 5 H 10 ] 2 have been previously reported, we synthesized seven [Bu i 2 AlR] 2 derivatives [R = NMe 2 , NPr n 2 ,NBu n 2 , NC 4 H 8 , NC 5 H 10 , NC 6 H 12 , and N(C 2 H 4 ) 2 NMe] by the reaction of Bu i 2 AlH with the corresponding secondary amines and one, [Bu i 2 AlNBu i 2 ] 2 , by the reaction of Bu i 2 AlCl with LiNBu i 2 . Also reported is the synthesis of the trimeric [Bu i 2 AlAsMe 2 ] 3 , which is an observed reaction product in the Me 2 AsNPr i 2 and Me 2 AsNBu i 2 systems.…”

Section: Introductionmentioning

confidence: 99%

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Reactivity of R₂AlH (R = Me, Buⁱ) with Selected Aminoarsines and Secondary Amines

et al. 1996

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Me2AlH and Bui 2AlH were reacted with a series of nine aminoarsines, Me2AsR (R = NMe2, NPrn 2, NPri 2, NBun 2, NBui 2, NC4H8, NC5H10, NC6H12, and N(C2H4)2NMe), in C6D6 at room temperature, and the reactions were monitored by 1H and 13C NMR spectroscopy. The relative rates for initial As−N bond cleavage and final product formation were dependent on the steric requirements of the alkyl groups attached to aluminum and nitrogen in the starting materials. Overall rates were slower with Bui 2AlH than with Me2AlH for a given aminoarsine. For most of the reactions, the predominant Al-containing products were the dimeric aminoalane compounds, [Me2AlR]2 and [Bui 2AlR]2. Although Al−N bond formation was the prefered mode of reaction, Al−As bond formation was also observed when the bulky Pri and Bui aminoarsine derivatives were used. The [Bui 2AlR]2 compounds were synthesized independently by the reaction of Bui 2AlH and the respective amine or, in the case of [Bui 2AlNBui 2]2, by the reaction of Bui 2AlCl and LiNBui 2. X-ray crystal structures were determined for the compounds [Me2AlNC6H12]2, [Me2AlN(C2H4)2NMe]2, [Bui 2AlNMe2]2, and [Bui 2AlN(C2H4)2NMe]2. All of the compounds have planar Al2N2 rings with the exception of [Bui 2AlN(C2H4)2NMe]2, which displays a puckered Al2N2 ring.

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Section: Resultssupporting

confidence: 65%

Section: Introductionmentioning

confidence: 99%

Reactivity of R₂AlH (R = Me, Buⁱ) with Selected Aminoarsines and Secondary Amines

et al. 1996

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“…26 Similar observations have been also been reported for the reactions of AlMe 3 with Me 2 AsNMe 2 , MeAs(NMe 2 ) 2 and As(NMe 2 ) 3 . 27,28 Therefore, it is likely that similar reactions and ligand rearrangements are taking place in the AACVD bubbler prior to deposition.…”

Section: Resultsmentioning

confidence: 99%

A solution based route to GaAs thin films from As(NMe₂)₃ and GaMe₃ for solar cells

et al. 2015

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The novel deposition of GaAs thin films on glass substrates from a solution based route involving the aerosol assisted chemical vapour deposition (AACVD) of As(NMe 2 ) 3 and GaMe 3 dissolved in toluene is reported. The gallium arsenide films were analysed by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), energy dispersive X-ray (EDX) analysis, X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. Powder XRD showed that cubic polycrystalline GaAs had been deposited with films grown at the higher temperatures having a Ga to As ratio of 1 : 1. EDX mapping, XPS depth profiling and SIMS showed that the films contained low levels of contaminants. The method described shows the formation of GaAs films with increasing crystallinity and stoichiometry reaching unity with increasing deposition temperature.

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“…An additional reaction for the Me 2 AlH/P(SiMe 3 ) 3 system at a 2:1 mol ratio was also carried out. The reactants were loaded into J Young NMR tubes at −115 °C using a previously published procedure …”

Section: Methodsmentioning

confidence: 99%

Reactivity of R₂AlH (R = Me, Buⁱ) and Me₃M (M = Al, Ga, In) toward the Silylphosphines P(SiMe₃)₃ and HP(SiMe₃)₂

et al. 1996

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2 species. The variable-temperature, multinuclear NMR study of the Me 2 AlH/ P(SiMe 3 ) 3 system indicated adduct formation at -90 °C and subsequent conversion to cyclic oligomeric [Me 2 AlP(SiMe 3 ) 2 ] n [Me 2 AlH] m species at -80 °C that ultimately produced [Me 2 -AlP(SiMe 3 ) 2 ] 2 . The reactivity of Bu i 2 AlH toward P(SiMe 3 ) 3 and HP(SiMe 3 ) 2 is much slower then that of Me 2 AlH. In the Bu i 2 AlH/HP(SiMe 3 ) 2 system, H 2 elimination is favored and [Bu i 2 -AlP(SiMe 3 ) 2 ] 2 and Bu i 2 AlP(SiMe 2 ) 2 ‚Bu i 2 AlP(H)SiMe 3 are formed. An X-ray structure analysis of [Bu i 2 AlP(SiMe 3 ) 2 ] 2 establishes the planarity of the (AlP) 2 core.Recently we reported the reactivity of Me 2 AlH with HP(SiMe 3 ) 2 , 26 wherein the preferred mode of reactivity is HSiMe 3 sas opposed to H 2 selimination. Transpho-

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Multinuclear NMR studies of the reactions of (Me3Al)2 with Me2AsNMe2, MeAs(NMe2)2 and As(NMe2)3

Cited by 17 publications

References 53 publications

Reactivity of R₂AlH (R = Me, Buⁱ) with Selected Aminoarsines and Secondary Amines

Reactivity of R₂AlH (R = Me, Buⁱ) with Selected Aminoarsines and Secondary Amines

A solution based route to GaAs thin films from As(NMe₂)₃ and GaMe₃ for solar cells

Reactivity of R₂AlH (R = Me, Buⁱ) and Me₃M (M = Al, Ga, In) toward the Silylphosphines P(SiMe₃)₃ and HP(SiMe₃)₂

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Multinuclear NMR studies of the reactions of (Me3Al)2 with Me2AsNMe2, MeAs(NMe2)2 and As(NMe2)3

Cited by 17 publications

References 53 publications

Reactivity of R2AlH (R = Me, Bui) with Selected Aminoarsines and Secondary Amines

Reactivity of R2AlH (R = Me, Bui) with Selected Aminoarsines and Secondary Amines

A solution based route to GaAs thin films from As(NMe2)3 and GaMe3 for solar cells

Reactivity of R2AlH (R = Me, Bui) and Me3M (M = Al, Ga, In) toward the Silylphosphines P(SiMe3)3 and HP(SiMe3)2

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Reactivity of R₂AlH (R = Me, Buⁱ) with Selected Aminoarsines and Secondary Amines

Reactivity of R₂AlH (R = Me, Buⁱ) with Selected Aminoarsines and Secondary Amines

A solution based route to GaAs thin films from As(NMe₂)₃ and GaMe₃ for solar cells

Reactivity of R₂AlH (R = Me, Buⁱ) and Me₃M (M = Al, Ga, In) toward the Silylphosphines P(SiMe₃)₃ and HP(SiMe₃)₂