tetrahydrofuran; germanium tetrachloride

in tetrahydrofuran; diethyl ether (N2); added dropwise a soln. of C2H3MgBr to a suspn. of Ge-compound; stirred for 1 h at 45°C; hydrolyzed; extracted with ether; washed with water; dried over MgSO4; evapd.;

in tetrahydrofuran a soln. of CH2CHMgCl allowed to stand for 24 h, the upper layer decantedto the reaction flask, a soln. of GeCl4 added at a temp. not exceeding 30°C, kept at 20-30°C for 6 h; treated with H2O, the aq. layer sepd., the org. layer washed (H2O), distd. fractionally;

magnesium in tetrahydrofuran byproducts: MgCl2; (1) vinyl chloride bubbled through a suspn. of Mg in an inert atmosphere, the react. initiated with 1,2-dibromoethane and performed at 55-60°C (25-30°C by the end); (2) a soln. of GeCl4 added dropwise at temp. not exceeding 30°C; kept at 20-30°C for 6 h; treated with H2O, the aq. layer sepd., the org. layer washed (H2O), distd. fractionally to give mixts.;