Neue oder verbesserte Synthesen für Germa- und Germa-sila-alkane und ihre chlorierten Vorstufen / New or Improved Syntheses for Germa- and Germa-sila-alkanes and their Chlorinated Precursors

Abstract

Reaction of germanium powder and Cl3SiCH2Cl at 350 °C yields the l-germa-3-silapropane Cl3SiCH2GeCl3, and (Cl3SiCH2)2GeCl2, in a “Direct Synthesis”. Cl3GeCH2CH2GeCl3 is obtained from HGeCl3 and C2H2 as a “Hydrogermylation” product. Addition of CH2=CHSiCl3 to HGeCl3 yields the 1-germa-4-silabutane Cl3SiCH,CH2GeCl3, and Cl3GeCH2C(GeCl3)=CH2 is obtained similarly from ClCH2C=CH and HGeCl3-NEt3. These Chlorogermanes or -germanes/silanes are converted into the corresponding germanes (silanes) by treatment with LiAlH4 in tetralin as a solvent in the presence of triethyl(benzyl)ammonium chloride. The products are isolated in high yields and identified by standard analytical techniques, including 73Ge NMR spectroscopy. Owing to their high volatility they are potential feed-stock gases for CVD experiments to generate a-GeC:H or a-Ge,Si,C:H materials.