三甲基(五甲基环戊二烯)钛合成路线 (共 5 条)
反应条件
in diethyl ether; hexane byproducts: LiCl; all manipulations carried out under dry Ar; soln. of LiMe in diethyl ether slowly added to an ice-cold suspension of Ti-compd. in hexane, mixt. left to reach room temp. with stirring for 4h; filtered, evapd., recrystn. (pentane, -78°C); elem. anal.;
参考文献
Mena, Miguel; Royo, Pascual; Serrano, Ricardo; Pellinghelli, Maria Angela; Tiripicchio, Antonio
Organometallics, 1989 , vol. 8, p. 476 - 482
反应条件
in benzene-d6 byproducts: CH4; Ti complex reacted with AlMe3 in C6D6 at room temp.; monitored by (1)H NMR spectra; variety of species obtained;
参考文献
Organometallics, , vol. 23, # 4 p. 836 - 845
反应条件
in toluene mixing of soln. of (C5Me5)TiMe((C5H9)7Si7O9(OSiMe3)O2) and AlMe3 (2 equiv.) in toluene in sealed ampule; heating to 60°C for 1 h; evapn. of all volatiles on vac. line at 60°C; condensing to activated charcoal colled with liq. N2; dissolving in C6D6 or C7D8; pouring into NMR tube; sealing; monitoring by NMR;
参考文献
Organometallics, , vol. 28, # 24 p. 6944 - 6956
反应条件
in toluene mixing of soln. of (C5Me5)TiMe(O(t-Bu))2 and AlMe3 (2 equiv.) in toluenein sealed ampule; heating to 100°C for 1 h; evapn. of all volatiles on vac. line at 60°C; condensing to activated charcoal colled with liq. N2; dissolving in C6D6 or C7D8; pouring into NMR tube; sealing; monitoring by NMR;
参考文献
Organometallics, , vol. 28, # 24 p. 6944 - 6956
反应条件
in toluene mixing of soln. of (C5Me5)TiMe((C5H9)7Si8O12O)2 and AlMe3 (2 equiv.) in toluene in sealed ampule; heating to 60°C for 1 h; evapn. of all volatiles on vac. line at 60°C; condensing to activated charcoal colled with liq. N2; dissolving in C6D6 or C7D8; pouring into NMR tube; sealing; monitoring by NMR;
参考文献
Organometallics, , vol. 28, # 24 p. 6944 - 6956