反应条件
in N,N,N',N',N'',N''-hexamethylphosphoric triamide; diethyl ether; pentane byproducts: LiCl; argon atmosphere; HMPA addn. to Li, stirring until soln. blue-grey, dropwise addn. of Me3GeCl soln. (Et2O), stirring (room temp., 3.5 h), germyllithium soln. addn. to SiCl4 soln. (pentane, -78°C), reaction mixt. stirring overnight at room temp.; acidic work-up, solvents removal (distn.), HMPA removal (dry column flash chromy., silica gel, pentane), (Me3Ge)2 and (Me3Ge)4Si sepn. by trap-to-trap distn. (room temp., 0.7 Torr), (Me3Ge)4Si purification by sublimation (62°C, 0.7 Torr);
参考文献
Canadian Journal of Chemistry, , vol. 70, # 12 p. 2884 - 2886
