in diethyl ether; anhydrous butyl ether using Schlenk techniques; charging of flask with PhLi in Bu2O under Ar, addn. of soln. of ZnCl2 in Et2O at -50°C, stirring for 3 h in thedark; centrifugation for 0.5 h at 2000 rpm, sepn. of soln., removal of solventunder reduced pressure at 50°C, sublimation (reduced pressure, 1 80°C);
magnesium; ethylene dibromide in diethyl ether bromobenzene is added to a stirred mixt. of Mg turnings and 1,2-dibromoethane, mixt. is warmed to 30°C, dry ether is added, mixt. is heated at reflux for 30 min, ZnCl2 (as etherate) is added, mixt. is heated at reflux for 2 h, then cooled;
参考文献
Australian Journal of Chemistry, , vol. 45, # 1 p. 121 - 134
in diethyl ether byproducts: LiCl; to soln. of MeCHCHCH2ZnCl in Et2O added soln. of PhLi in Et2O at -10 °C; filtered, evapd. (20 °C, 0.1 Torr), distd. at 37-40 (0.0001 Torr), then sublimed at 70 .gedree.C (0.0001 Torr); elem. anal.;
参考文献
Journal of Organometallic Chemistry, , vol. 289, p. 1 - 8
