Synthetic and Structural Studies of Donor-Functionalized Alkoxy Derivatives of Gallium
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- 作者：Caroline E. Knapp ; David Pugh ; Paul F. McMillan ; Ivan P. Parkin ; Claire J. Carmalt
- 刊名：Inorganic Chemistry
- 出版年：2011
- 出版时间：October 3, 2011
- 年：2011
- 卷：50
- 期：19
- 页码：9491-9498
- 全文大小：905K
- 年卷期：v.50,no.19(October 3, 2011)
- ISSN：1520-510X
文摘
The synthesis of a range of alkyl/chloro-gallium alkoxide and amido/alkoxide compounds was achieved via a series of protonolysis and alcoholysis steps. The initial reaction involved the synthesis of [Me(Cl)Ga{N(SiMe3)2}]2 (1) via methyl group transfer from the reaction of GaCl3 with two equivalents of LiN(SiMe3)2. Reaction of 1 with varying amounts of ROH resulted in the formation of [Me(Cl)Ga(OR)]2 (2, R = CH2CH2OMe; 3, CH(CH3)CH2NMe2), [Me(Cl)Ga{N(SiMe3)2}(渭2-OR)Ga(Cl)Me] (4, R = CH2CH2NMe2), or [MeGa(OR)2] (5, R = CH(CH3)CH2NMe2). Compound 4 represents an intermediate in the formation of dimeric complexes, of the type [Me(Cl)Ga(OR)]2, when formed from compound [Me(Cl)Ga{N(SiMe3)2}]2. A methylgallium amido/alkoxide complex [MeGa{N(SiMe3)2}(OCH2CH2OMe)]2 (6) was isolated when 2 was further reacted with LiN(SiMe3)2. In addition, reaction of 2 with HOtBu resulted in a simple alcohol/alkoxide exchange and formation of [Me(Cl)Ga(OtBu)]2 (7). In contrast to the formation of 1, the in situ reaction of GaCl3 with one equivalent of LiN(SiMe3)2 yielded [Cl2Ga{N(SiMe3)2}]2 in low yield, where no methyl group transfer has occurred. Reaction of alcohol with [Cl2Ga{N(SiMe3)2}]2 was then found to yield [Cl2Ga(OR)]2 (8, R = CH2CH2NMe2), and further reaction of 8 with LiN(SiMe3)2 yielded the gallium amido alkoxide complex, [ClGa{N(SiMe3)2}(OR)]2 (9, R = CH2CH2NMe2), similar to 6. The structures of compounds 4, 5, 7, and 8 have been determined by single-crystal X-ray diffraction.
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