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
Amor, J. I.; Burton, N.C.; Cuenca, T.; Gomez-Sal, P.; Royo, P.
Journal of Organometallic Chemistry, 1995 , vol. 485, # 1-2 p. 153 - 160
1: With zirconocene dichloride; magnesium in tetrahydrofuran T=0 - 21°C; 5 h; Inert atmosphere; 2: With hydrogenchloride in tetrahydrofuran; water regioselective reaction;
参考文献
D'yakonov; Timerkhanov; Tyumkina; Dzhemilev
Russian Chemical Bulletin, 2009 , vol. 58, # 12 p. 2456 - 2464
Izv. Akad. Nauk, Ser. Khim., 2009 , # 12 p. 2378 - 2385,8
1: With zirconocene dichloride; magnesium in tetrahydrofuran T=0 - 21°C; 5 h; Inert atmosphere; 2: With hydrogenchloride in tetrahydrofuran; water regioselective reaction;
参考文献
D'yakonov; Timerkhanov; Tyumkina; Dzhemilev
Russian Chemical Bulletin, 2009 , vol. 58, # 12 p. 2456 - 2464
Izv. Akad. Nauk, Ser. Khim., 2009 , # 12 p. 2378 - 2385,8
in further solvent(s) (Ar); using Schlenk techniques; mixing of EtAlCl2 and TBP; evolution of gas;
参考文献
Bulgakov, Ramil G.; Kuleshov, Sergei P.; Zuzlov, Aleksei N.; Mullagaleev, Ildar R.; Khalilov, Leonard M.; Dzhemilev, Usein M.
Journal of Organometallic Chemistry, 2001 , vol. 636, # 1-2 p. 56 - 62