Synthesis and Structural Characterization of a Terminal Hydroxide Containing Alumoxane via Hydrolysis of Aluminum Hydrides

Ying Peng; Guangcai Bai; Huiqing Fan; Denis Vidovic; Herbert W. Roesky; Jörg Magull

doi:10.1021/ic0351803

journal article Jan 30, 2004

Synthesis and Structural Characterization of a Terminal Hydroxide Containing Alumoxane via Hydrolysis of Aluminum Hydrides

Ying Peng

Guangcai Bai Huiqing Fan

Denis Vidovic Herbert W. Roesky

Jörg Magull

Inorganic Chemistry Vol. 43 No. 4 pp. 1217-1219 · American Chemical Society (ACS)

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Synthesis of2: tert-Butyl isocyanate (0.14 mL, 1.2 mmol) was added by syringe to LAlH2(0.55 g, 1.25 mmol) in toluene (20 mL). The solution was refluxed for 1 h. After removal of all the volatiles the residue was recrystallized from pentane. The resulting solution was concentrated to ca. 5 mL and kept at 0 °C to afford colorless crystals. Yield: 68% (0.44 g). Mp: 141−143 °C. EI-MS: m/z(%) 545 (38) [M+], 544 (100) [M+− H].1H NMR (300.13 MHz, C6D6): δ 7.54 (s, 1H, CHN), 7.12−7.15 (m, 6H, Ar−H), 5.09 (s, 1H, γ-H), 3.41 (sept, 4H, CHMe2), 1.55 (s, 6H,Me), 1.38 (d, 6H,3JH-H= 6.8 Hz, CHMe2), 1.28 (d, 6H,3JH-H= 6.7 Hz, CHMe2), 1.18 (d, 6H,3JH-H= 6.8 Hz, CHMe2), 1.12 (d, 6H,3JH-H= 6.9 Hz, CHMe2), 1.07 (s, 9H,tBu). IR (Nujol mull, cm-1): 1868 (ν̃Al-H). Calcd for C34H52AlN3O (545.78): C, 74.82; H, 9.60; N, 7.70. Found: C, 75.03; H, 9.51; N, 7.83.

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Details

Published: Jan 30, 2004
Vol/Issue: 43(4)
Pages: 1217-1219

Authors

Y

Ying Peng