n-BuLi in not given n-BuLi in hexane added dropwise to ligand in Et2O at 0°C; warmed to room temp.; stirred overnight; filtered; ppt. washed (Et2O); dried invac.; added to ZrCl4; C5H5Li added; mixt. of three Zr complexes obtaine d; sepd. by fractional crystn.; (C5H5)(C5HMe2Ph2)ZrCl2 contg. (C5H5)2ZrCl2 impurity obtained; detd. by NMR spectra;
参考文献
Journal of Organometallic Chemistry, , vol. 694, # 2 p. 173 - 178
in benzene-d6 Irradiation (UV/VIS); a soln. of complexes, molar ratio Ph2ZrCp2:(styryl)ZrClCp2 1:2 was irradiated for 16 h at 20°C in a sealed NMR tube; not sep.;
in benzene-d6 byproducts: Ph3CCH3; N2 glovebox; Zr complex was treated with Ph3CCl (1-1.1 equiv.) in benzene-d6 at 60°C for 18 h; NMR monitoring; not isolated;
