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The synthesis of higher silicon hydrides containing Ph3Ge groups was accomplished in excellent yields on a multigram scale starting from neopentasilane using an easy-to-perform reaction pathway. Reactivity studies showed that the obtained products cleanly can be transformed with MeLi to the corresponding lithium silanides, which are valuable educts for further derivatization. Treatment with CF3SO3H/iBu2AlH, on the other hand, afforded several species arising from Ge−Ph and Ge−Si bond scission.
Mixed Si/Ge hydrides SixGeyHz are valuable precursors for the deposition of binary Si–Ge alloys. This work describes the synthesis and full characterization of the previously unknown germaisotetrasilane Ph3GeSi(SiH3)3 (2) on a multigram scale from the reaction of the lithium silanide LiSi(SiH3)3 with Ph3GeCl. The stability of the Si–Ge bond in 2 versus electrophiles and nucleophiles has been investigated with the primary aim of developing new approaches to mixed sila-H-germanes (H3Ge)xSi(SiH3)4–x. With 1 equiv of MeLi, 2 reacted cleanly under cleavage of one Si–Si bond to give Ph3GeSi(SiH3)2Li, which is a valuable synthon for further derivatization. In contrast, the dephenylation reaction of 2 with 1 or 2 equiv of CF3SO3H/iBu2AlH proceeded much less selectively and afforded the desired Ph/H-germasilanes Ph2HGeSi(SiH3)3 and PhH2GeSi(SiH3)3 along with considerable amounts of Si–Ge scission products.
|حجم فایل||912 B|