in dichloromethane under N2, Schlenk techniques; Sn-Si compd. added dropwise to suspn. of TaCl5 in CH2Cl2 at 0°C, mixt. warmed to room temp.; volatiles removed under vac., light petroleum added to residue, cooled to -30°C; elem. anal.;
in dichloromethane byproducts: (CH3)2NC2H4N(CH3)2*HCl; under N2, Schlenk techniques; Sn-Si compd. added dropwise to suspn. of TaCl5 in CH2Cl2 at 0°C, mixt. warmed to room temp., volatiles removed under vac., residue dissolved in light petroleum, Me2NC2H4NMe2 addedat 0°C; crystd. at -30°C; elem. anal.;
in diethyl ether; hexane under N2 atm. slurry TaCl5 in hexane at -20°C was treated dropwise with Me3SiCH2MgCl in Et2O, solvent was removed in vacuo, residue was taken up in hexane at 0°C and filtered, PMe3 was added and heated to 50°C for 1 h; soln. was filtered, concd. and cooled to -20°C;
参考文献
Diminnie, Jonathan B.; Blanton, Jaime R.; Cai, Hu; Quisenberry, Keith T.; Xue, Ziling
Organometallics, 2001 , vol. 20, # 8 p. 1504 - 1514
