in diethyl ether; cyclohexane to 1-bromooctane (1 mmol) and TMTH (1 mmol) in Et2O at 0°C added LDA (1 mmol, in cyclohexane) under Ar, stirred for 20 min, quenched; analyzed by GLPC;
in hexane; cyclohexane 1-bromooctane (1 equiv.) and TMTH (2 equiv.) in hexane cooled to 0°C under Ar, LDA (1 equiv., 1.6 M soln. in cyclohexane) dropped in, stirred for 20-25 min at room temp., quenched with water; analyzed by GC (after quenching), NMR (before quenching);
in tetrahydrofuran TMTH (1.10 mmol) and 1-bromooctane (1.10 mmol) in THF cooled to 0°C under Ar, MeLi (1.10 mmol) in THF added, stirred for 15 min at room temp., hydrolyzed with water; H2 collected with gas measuring device, GC analysis of org. layer;
in diethyl ether TMTH (1.00 mmol) and 1-bromooctane (1.00 mmol) in Et2O cooled to 0°C under Ar, MeLi (1.00 mmol, 1.00 M soln. in Et2O) added, stirred for 15 min at room temp., hydrolyzed with water; H2 collected with gas measuring device, GC analysis of org. layer;
in hexane; cyclohexane byproducts: LiBr; to soln. of 1-bromooctane (1.0 mmol) and TMTH (1.0 mmol) in hexane at 0°C added LDA (1.00 mmol, 1.6 M soln. in cyclohexane) under Ar, react. time 10 min; analyzed by GLPC;
in hexane; cyclohexane byproducts: LiBr; to soln. of 1-bromooctane (1.0 mmol) and TMTH (1.0 mmol) in hexane at 0°C added LDA (0.50 mmol, 1.6 M soln. in cyclohexane) under Ar, react. time 10 min; analyzed by GLPC;
参考文献
Reimann, Werner; Kuivila, Henry G.; Farah, Dan; Apoussidis, Theodorus
Organometallics, 1987 , vol. 6, p. 557 - 565
in further solvent(s) equilibrium in azoisobutyric acid dinitrile at 40°C; examination with NMR-spectroscopy;;
参考文献
Creemers, H. M. J. C.; Verbeek, F.; Noltes, J. G.
Journal of Organometallic Chemistry, 1967 , vol. 8, p. 469 - 477
Full Text Show Details
Gmelin Handbook: Sn: Org.Verb.4, 1.2.1.1.1.4.6, page 17 - 18
in neat (no solvent) inert atmosphere (N2, Ar or high vac.), room temperature, equimolar amts. of halosilane/tinhydride, reactn. time 3 h; not isolated; IR spectroscopy (identified 85percent SiCl3H, 5percent SiH4 and 5percent SiCl4 in product mixt.);
参考文献
D'Errico, John J.; Sharp, Kenneth G.
Inorganic Chemistry, 1989 , vol. 28, p. 2177 - 2180
