ZUR CHEMIE VON t-BUTYLGERMANIUM-HALOGENIDEN UND -CHALKOGENIDEN

Article abstract of DOI:10.1016/S0022-328X(00)84322-3

Upon reaction with an excess of t-C4H9Li GeCl4 gives <(t-C4H9)2GeH>2 (I) and with 2 equivalents of t-C4H9Li it gives (t-C4H9)2GeCl2 (II) together with rearranged and condensated products (III, IV, V) and polycondensates.The reaction with 3 molar equivalents of t-C4H9Li gives predominantly (t-C4H9)3GeCl (VI) with a minor amount of I.Also (t-C4H9)2GeH2 (VII) could be isolated.In the presence of triethylamine from the reaction of II with H2S, (t-C4H9)2Ge(SH)2 (VIII) is obtained, which readily condenses to give cyclotetra-t-butyl-1,3-dithia-2,4-digermane (IX).IX can be also obtained in high yields from the reaction of I and sulfur, and from II and KHS in the presence of 18-crown-6, with cyclotetra-t-butyl-1,2,4-trithia-3,5-digermane (X) as a byproduct.X is the main product in the reaction of II and H2S in the presence of imidazole.From I and selenium or tellurium the corresponding 4-membered ring compounds XI and XII are obtained, with the 5-membered ring compound XIII as a byproduct of the reaction with selenium.The compounds are characterized spectroscopically (MS, 1H-NMR, and partly IR) and for those which have been separated in a pure state also by analyses.An X-ray structure determination has been performed for IX.