sodium in 1,4-dioxane byproducts: NaCl; a soln. of o-ClC6H4OSnBu3 in dry dioxane was added to a suspn. of Na (10percent excess) within 10-15 min under inert atmosphere, mixt. was stirred for 8 h at 20°C, an excess of Me3SiCl added, stirred for 15 h at 20°C; reaction mixt. was filtered and distilled; elem. anal. for o-Bu3SnC6H4OSiMe3;
参考文献
Journal of Organometallic Chemistry, , vol. 243, # 1 p. 1 - 8
lithium or magnesium in tetrahydrofuran a soln. of o-BrC6H4OSnBu3 in dry THF was added to a suspn. of Li or Mg under inert atmosphere, mixt. was stirred at 35°C, an excess of Me3SiCl added, stirred at the same temp.; reaction mixt. was filtered and distilled;
参考文献
Journal of Organometallic Chemistry, , vol. 243, # 1 p. 1 - 8
in tetrahydrofuran Electrolysis; electrolysis carried out galvanostatically at 25-28°C in an atm.of dry N2, electrolyte 0.4 M LiClO4/THF; hexane added to electrolyte, ppt. filtered off, filtrate analyzed for product by GC, Bu3SnSiMe3 isolated in pure by chromy.;
in diethyl ether byproducts: NaCl; addn. of Me3SiCl to a soln. of Na(Et3BCCCHCMe2), 3 h boiling, filtration, solvent removed (760 Torr, than in vacuo), distillation at 0.001 Torr; elem. anal.;
