tert.-butyl lithium; methyl iodide in tetrahydrofuran; pentane byproducts: BuH, LiI; under N2 or Ar, addn. of t-BuLi in pentane to a soln. of the germyl compd. in THF at -40°C, stirring, 40 min, -40°C, formation of the dilithium, addn. of an excess of MeI at -40°C, ambient temp., 30 min at 20°C, hydrolysis; extn., concg. under vac., recrystn. (pentane), detn. by 13C and 1H NMR;

water; tert.-butyl lithium; methyl iodide in tetrahydrofuran; pentane byproducts: BuH, LiI; under N2 or Ar, addn. of t-BuLi in pentane to a soln. of the digermyl compd. in THF at -40°C, stirring for 30 min, -40°C, addn. of an excess of MeI, warming to ambient temp., 30 min at 20°C, hydrolysis; extn., concg. under vac., 1H NMR, not isolated;

in tetrahydrofuran byproducts: LiCl, AlH3; to Ge complex (0.209 mmol) soln. added suspn. of LiAlH4 (0.416 mmol), stirred under N2 for 18 h at 25°C; solvent removed in vac., washed with benzene, dried in vac.;

in pentane byproducts: LiH, isobutane; inert atmosphere; addn. of t-BuLi soln. in pentane to Ph2GeH2 soln. in Et2NMe (-40°C), stirring (20°C, 14 h); hydrolysis, extn., concentration, crystn. (Et2O/MeOH 4:1); slightly impure;

in tetrahydrofuran; diethyl ether inert atmosphere; -70°C, 1 h; evapn. (vac.), washing (pentane), evapn.; NMR spectroscopy;

water byproducts: LiH; Addn. of Et3N gives different intermediates depending on react. time. The react. is finished after 5 min (addn. of H2O).; Isolated after hydrolysis.;

in toluene byproducts: H2; under Ar or N2; H2GePh2 (5 equiv.) and Pt complex in toluene heated at 90°C for 48 h; solvent evapd. to dryness; recrystd. from toluene-hexane; elem. anal.;

1: toluene 2: toluene 3: toluene View Scheme

1: toluene 2: acetone 3: tetrahydrofuran View Scheme

in tetrahydrofuran inert atmosphere; -20°C (20 min), then stirring (20°C, 2 h); hydrolysis, extn., concentration (vac.);