magnesium in N,N-dimethyl-formamide byproducts: Mg(2+); Electrolysis; electrolysis carried out in a single-compartment cell at room temp., starting materials dissolved in DMF containing KBr or n-Bu4NBr, solvent andexcess B(OCH3)3 evaporated under vacuum, medium hydrolysed at 0° C with an HCl or H2SO4 soln.; extraction with Et2O (3 x 20 ml if the solvent evaporated or 3 x 60 ml otherwise), organic phase dried over sodium or magnesium sulfate and concentrated under vacuum, side product phenol formation avoided by work-up under inert atmosphere;
参考文献
Laza, Carine; Dunach, Elisabet; Serein-Spirau, Francoise; Moreau, Joel J. E.; Vellutini, Luc
New Journal of Chemistry, 2002 , vol. 26, # 4 p. 373 - 375
1: With manganese; NiCl2((PPh3)P)2; tetraethylammonium iodide; triphenylphosphine in 1,3-dimethyl-imidazolidin-2-one T=25°C; P=760.051 Torr; 20 h; 2: With hydrogenchloride; water in diethyl ether T=20°C; 0.166667 h;
参考文献
Fujihara, Tetsuaki; Nogi, Keisuke; Xu, Tinghua; Terao, Jun; Tsuji, Yasushi
Journal of the American Chemical Society, 2012 , vol. 134, # 22 p. 9106 - 9109
