(五甲基环戊二烯基)三氯化钛(IV)合成路线 （共 17 条）
反应条件
in toluene under Ar atm. using Schlenk techniques; recrystd. from toluene/pentane;
参考文献
Kim, Youngjo; Han, Yonggyu; Hwang, Jeong-Wook; Kim, Myong Woon; Do, Youngkyu
Organometallics, 2002 , vol. 21, # 6 p. 1127 - 1135
反应条件
hydrogenchloride in tetrahydrofuran; diethyl ether; pentane stirring a suspension in THF at room temp. for 12 h, after removal of THF in vac. intermediate Ti compd. was oxidized with HCl soln.; evapn. of solvent, sublimation (120°C/0.001mmHg), elem. anal.;
参考文献
Blenkers, J.; Meijer, H. J. de Liefde; Teuben, J. H.
Journal of Organometallic Chemistry, 1981 , vol. 218, # 3 p. 383 - 394
反应条件
in toluene N2-atmosphere; excess Me3SiCl, stirring at room temp. for 3 h; removal of volatiles;
参考文献
Yu, Peihua; Pape, Thomas; Uson, Isabel; Said, Musa A.; Roesky, Herbert W.; Montero, Mavis L.; Schmidt, Hans-Georg; Demsar, Alojz
Inorganic Chemistry, 1998 , vol. 37, # 20 p. 5117 - 5124
反应条件
HCl in toluene (Ar), HCl gas (1 atm static pressure) added to a soln. of the complex, stirred for 1 h; excess HCl pumped away, toluene removed under vacuum, hexane added, stirred for a few minutes, filtered, (C5(CH3)5)2TiCl2 pptd., filtrate evapd. under vacuum, (C5(CH3)5)TiCl3 crystd., elem. anal.;
参考文献
Organometallics, , vol. 4, p. 550 - 553
反应条件
in dichloromethane byproducts: HCl; under N2, Schlenk technique; soln. of C5Me5 in CH2Cl2 added dropwise to soln. of TiCl4 in CH2Cl2 at room temp., mixt. heated at 80°C under stirring overnight; ppt. filtered off, solvent removed, residue dried at 100°C under vac.; elem. anal.;
参考文献
Zhang, Yuetao; Mu, Ying
Organometallics, 2006 , vol. 25, # 3 p. 631 - 634
反应条件
in toluene Dropwise addn. of TiCl4 in toluene to soln. of C(CH3)5Si(CH3)3 in toluene (N2), stirring (2 h, color change from red-orange to red).; Evapn. of solvent and byproduct (vacuum), washing of crystals (pentane), dried (vacuum), elem. anal.;
参考文献
Llinas, Gerardo Hidalgo; Mena, Miguel; Palacios, Federico; Royo, Pascual; Serrano, Ricardo
Journal of Organometallic Chemistry, 1988 , vol. 340, p. 37 - 40
反应条件
in toluene 1:1 react. at 30°C;
参考文献
Yasuda, Hajime; Yamamoto, Hitoshi; Yokota, Kiyohiko; Nakamura, Akira
Chemistry Letters, 1989 , p. 1309 - 1312
参考文献
Organometallics, , vol. 19, # 14 p. 2816 - 2819
反应条件
in toluene (inert atmosphere); slow addn. of AlEtCl2 in toluene at -78°C toa soln. of Ti complex in toluene, stirring (low temp., 2 h); quenching (pyridine), warming to room temp., removal of volatiles (vac.), washing (hexane), mixing the residual gum with toluene, isoln. of theproduct from hexane and toluene solns.; yield almost quantitative;
参考文献
Journal of Organometallic Chemistry, , vol. 485, # 1-2 p. 153 - 160
反应条件
in toluene TiCl4 and Yb-compound ratio 2:1, 30°C;
参考文献
Chemistry Letters, , p. 1309 - 1312
