in 1,4-dioxane; diethyl ether soln. of Me2Mg in Et2O/dioxane was added to soln. of Zr complex in Et2O;mixt. was stirred overnight; solvent removed (vac.); dissolved in C6H6; filtered; washed (C6H6); filtrate evapd. (vac.); washed (hexanes); dried (vac.);
参考文献
Petros, Robby A.; Camara, James M.; Norton, Jack R.
Journal of Organometallic Chemistry, 2007 , vol. 692, # 21 p. 4768 - 4773
in tetrahydrofuran
byproducts: CH3SCH2MgCH3; under anaerobic conditions, in NMR tube; Sn compd., Mg compd. (molar ratio 1:1) in THF, SnMe4 (internal standard) and THF mixed; reacted for 12 d; not isolated; monitored by (119)Sn NMR spectra; 10percent conversion;
in tetrahydrofuran; diethyl ether
byproducts: C6H5SCH2MgCH3; under anaerobic conditions, in NMR tube; Sn compd., Mg compd. (molar ratio 1:1) in Et2O, SnMe4 (internal standard) and THF mixed; reacted for 9 d; not isolated; monitored by (119)Sn NMR spectra; > 95percent conversion;
in tetrahydrofuran
byproducts: C6H5S(O)2CH2MgCH3; under anaerobic conditions, in NMR tube; Sn compd., Mg compd. (molar ratio 1:1) in THF, SnMe4 (internal standard) and THF mixed; reacted for 1 h; not isolated; monitored by (119)Sn NMR spectra; > 95percent conversion;
in tetrahydrofuran; diethyl ether
byproducts: CH3S(O)2CH2MgCH3; under anaerobic conditions, in NMR tube; Sn compd., Mg compd. (molar ratio 1:1) in Et2O, SnMe4 (internal standard) and THF mixed; reacted for 1 h; not isolated; monitored by (119)Sn NMR spectra; > 95percent conversion;
in tetrahydrofuran; diethyl ether
byproducts: C6H5S(O)CH2MgCH3; under anaerobic conditions, in NMR tube; Sn compd., Mg compd. (molar ratio 1:1) in Et2O, SnMe4 (internal standard) and THF mixed; reacted for 1 h; not isolated; monitored by (119)Sn NMR spectra; > 95percent conversion;
in tetrahydrofuran; hexane
byproducts: Me2PCH2MgMe, LiCH2PMe2; under anaerobic conditions; n-BuLi (0.1-0.2 equiv.) in n-hexane added at-78°C to Sn compd. (1 equiv.) in n-hexane, stirred at room temp. for 15 min; MgMe2 (1 equiv.) in THF added at -78°C; stirred for 30 min; warmed to room temp.; 4 d; not isolated; identified by (119)Sn NMR spectra; >95percent conversion;
in tetrahydrofuran; hexane
byproducts: Me2NCH2MgMe, LiCH2NMe2; under anaerobic conditions; n-BuLi (0.07-0.1 equiv.) in n-hexane added at -78°C to Sn compd. (1 equiv.) in n-hexane, stirred at room temp. for 15 min; MgMe2 (1 equiv.) in THF added at -78°C; stirred for30 min; warmed to room temp.; 1 d; not isolated; identified by (119)Sn NMR spectra; >95percent conversion;
