rac-二甲基硅基双(1-茚基)二氯化锆合成路线 (共 4 条)
反应条件
trimethylstannyl chloride in tetrahydrofuran; diethyl ether inert atmosphere; addn. of Me3SnCl to Li-salt in Et2O at -40°C, warming to room temp., evapn., addn. of ZrCl4 suspn. in THF, stirring (80°C, 4 h); evapn. (80-90°C, 1 torr), recrystn. or washing;
参考文献
Nifantev, Ilya E.; Ivchenko, Pavel V.
Organometallics, 1997 , vol. 16, p. 713 - 715
反应条件
methylaluminoxane in benzene-d6 under Ar, standard Schlenk techniques; solid dichloride Zr complex mixedwith 1 equiv. of Cp2ZrClMe; dissolved in benzene-d6; a minute amt. of s olid methylaluminoxane added; equil. reached within several min; not isolated; monitored by (1)H NMR spectra;
参考文献
Weiser, Ulrich; Babushkin, Dimitrii; Brintzinger, Hans-Herbert
Organometallics, 2002 , vol. 21, p. 920 - 923
反应条件
methylaluminoxane in benzene-d6 under Ar, standard Schlenk techniques; solid dichloride Zr complex mixedwith 1 equiv. of (indenyl)2ZrClMe; dissolved in benzene-d6; a minute am t. of solid methylaluminoxane added; equil. reached within several min; not isolated; monitored by (1)H NMR spectra;
参考文献
Weiser, Ulrich; Babushkin, Dimitrii; Brintzinger, Hans-Herbert
Organometallics, 2002 , vol. 21, p. 920 - 923
反应条件
in diethyl ether meso-Me2Si(1-indenyl)2ZrCl2 suspended in Et2O, cooled at -78°C, 2equiv. of CH3Li in Et2O added, after 30 min mixt. slowly warmed to room temp., stirred for 4 h; solvent removed under reduced pressure, residue extracted with anhydroustoluene, concd., cooled to -20°C; elem. anal.;
参考文献
Melillo, Gianluca; Izzo, Lorella; Centore, Roberto; Tuzi, Angela; Voskoboynikov, Alexander Z.; Oliva, Leone
Journal of Molecular Catalysis A: Chemical, 2005 , vol. 230, # 1-2 p. 29 - 33