Reduction of R₃Ga with Alkali Metals in Aromatic SolventsFormation of R₃GaAr^-and R₃GaH^- 1

Abstract

Reduction of trialkylgallium compounds (R3Ga) in benzene with alkali metals forms R3GaPh- and R3GaH- anions in addition to the expected R4Ga- anions. The portion of the product consisting of R3GaPh- and R3GaH- decreases as R is changed in the series sec-butyl > isobutyl > ethyl > methyl. Only R4Ga- is observed when the reducing agent is Li instead of Na/K alloy, K, or Cs. Reductions in a monoalkylbenzene form R3Ga(m-alkylphenyl)- and R3GaH-. 1H and 13C NMR spectra of s-Bu3Ga, s-Bu4Ga-, s-Bu3GaPh-, and s-Bu3GaH- show a discrete absorption for each diastereomer for some groupings.

Selective Grafting of Ga(i-Bu)3 on the Silanols of Mesoporous H-ZSM-5 by Surface Organometallic Chemistry

“…These assignments are in agreement with those reported elsewhere. 51 In agreement with the 1 H NMR spectrum, weak signals for trapped pentane molecules are observed at 34.6 and 12.6 ppm. 53 The 27 Al MAS and 1 H− 27 Al HMQC MAS NMR spectra of Ga(i-Bu) 3 /meso-H-ZSM-5 250 are similar to those of the meso-H-ZSM-5 250 starting material (Figures 6a and 6c, respectively).…”

“…For comparison, the 1 H solution NMR spectrum of Ga(i-Bu) 3 consists of peaks at 2.06 (CH), 1.00 (CH 3 ), and 0.74 ppm (CH 2 ). 51 Protons associated with the Brønsted acidic sites and extraframework aluminum OH are visible in the spectrum of Ga(i-Bu) 3 /meso-H-ZSM-5 250 at 4.2 and 2.7 ppm, respectively (the former being slightly shifted compared to the parent material, at 4.0 ppm). No signal for residual silanols was detected, although it may contribute to intensity on the low field side of the methyl peak (0.9 ppm).…”

Synthesis and Structural Characterization of β‐Ketoiminate‐Stabilized Gallium Hydrides for Chemical Vapor Deposition Applications

“…The absence of any resonances corresponding to the presence of the pro‐ligands (in particular that of the NH protons) within the 1 H NMR spectrum confirmed that the reaction had gone to completion. Peaks at −0.38 ppm correspond to the organometallic methyl protons, which show a slight upfield shift with respect to the unreacted starting material GaMe 3 (−0.18 ppm) 31. Mass spectrometry of 5 confirmed the formation of the bimetallic product by the detection of a fragment at m / z 419, corresponding to the molecular ion with loss of a CH 3 group.…”

Cationic Dialkyl Metal Compounds of Group 13 Elements (E = Al, Ga, In) Stabilized by the Weakly Coordinating Dianion [B12Cl12]2–

“…Me 3 Al (2.0 M in hexane, Aldrich) and Et 3 Al (ABCR, 93%) are commercially available and were used as received. [Ph 3 C] 2 [B 12 Cl 12 ], 16 Et 3 In, 38 and Et 3 Ga 3 (OEt) 39 were prepared by published procedures. IR spectra were recorded on a Nicolet Magna 760 IR spectrometer equipped with a diamond or ZnSe ATR attachment.…”