diethyl ether

copper in diethyl ether addn. of CH2N2 to mixt. of GeCl4 with little Cu-powder at -60°C (stirring), standing at -60°C for 2 h, slow warming to room temp.,solvent removal, addn. of excess MeMgBr (in Et2O), refluxing for 10 h; addn. of satd. aq. NH4Cl, washing aq. layer (Et2O), drying combined org.layers (MgSO4), solvent removal, fractional distn.;

in diethyl ether (N2); dropwise addn. (1 h) of a soln. of methyllithium into the soln. of GeCl3CH2Cl at -70 °C under vigorous stirring; addnl. stirring (1.5 h); then standing the mixt. until room temp. was reached and addnl. stirring for 16 h;; filtration; then distg. the solvent off from the filtrate; vacuum distn.;

in neat (no solvent) heating in an autoclave, 125°C, 4h; chromy.; elem. anal.;

anthracene; magnesium; methyl iodide in tetrahydrofuran; diethyl ether Mg/anthracene/MeI in THF stirred at room temp. for 2 h; Me3GeCH2Cl in THF added dropwise; stirred at room temp. for 16 h; DPPA in Et2O added slowly at -15°C; stirred at -10°C for 1 h, then at room temp. for 3 h;; added to pentane/ice; ppt. washed with pentane; organic phase concd.; distd.;;