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摘要
The quantitative conversion of the tertiary stannane (n-Bu)(3)SnH (2) into (n-Bu)(6)Sn(2) (4) was achieved by heating the neat hydride material under low pressure or under closed inert atmosphere conditions. A 31% conversion of Ph(3)SnH (3) to Ph(6)Sn(2) (5) was also observed under low pressure; however, under closed inert atmosphere conditions afforded Ph(4)Sn (6) as the major product. A mixed distannane, (n-Bu)(3)SnSnPh(3) (7), can also be prepared in good yield utilizing an equal molar ratio of 2 and 3 and the same reaction conditions used to prepare 4. This solvent-free, catalyst-free route to distannanes was extended to a secondary stannane, (n-Bu)(2)SnH(2) (8), which yielded evidence (NMR) for hydride terminated distannane H(n-Bu)(2)SnSn(n-Bu)(2)H (9), the polystannane [(n-Bu)(2)Sn](n) (10), and various cyclic stannanes [(n-Bu) (2)Sn](n=5),(6) (11, 12). Further evidence for 10 was afforded by gel permeation chromatography (GPC) where a broad, moderate molecular weight, but highly dispersed polymer, was obtained (M(w) = 1.8 x 10(4) Da, polydispersity index (PDI) = 6.9) and a characteristic UV-vis absorbance (lambda(max)) of approximate to 370 nm observed.
- 出版日期2010-10
