in neat (no solvent) inert atmosphere (N2, Ar or high vac.), room temperature, equimolar amts. of halosilane/tinhydride, reactn. time 36 h; not isolated; IR spectroscopy (identified 25-30percent SiCl3H, 15percent SiCl2H2 and 10percent SiH4 in product mixt.);
参考文献
D'Errico, John J.; Sharp, Kenneth G.
Inorganic Chemistry, 1989 , vol. 28, p. 2177 - 2180
in neat (no solvent) inert atmosphere (N2, Ar or high vac.), room temperature, two equiv. of tinhydride, reactn. time 2 h; not isolated; IR spectroscopy (identified 35-40percent SiCl3H, 40percent SiH4 and 10percent SiCl2HBr in product mixt.);
参考文献
D'Errico, John J.; Sharp, Kenneth G.
Inorganic Chemistry, 1989 , vol. 28, p. 2177 - 2180
in neat (no solvent) condensing of equimolar amts. of tinhydride and SiClHBr2 (trace of SiCl2HBr present) into cold finger, reaction at room temp. (30 min); further products; not isolated; IR spectroscopy;
参考文献
D'Errico, John J.; Sharp, Kenneth G.
Inorganic Chemistry, 1989 , vol. 28, p. 2177 - 2180
in not given byproducts: (CH3)2Sn(CHCF2)2, (CH3)2Sn(CFCHF)2, CF2CHF; reaction in darkness at 70°C;;
参考文献
Beveridge, A. D.; Clark, H. C.; Kwon, J. T.
Canadian Journal of Chemistry, 1966 , vol. 44, p. 179 - 189
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Gmelin Handbook: Sn: Org.Verb.4, 1.2.1.1.1.4.4, page 15 - 16
n-butyllithium in hexane n-BuLi (1.50 mmol, 2.40 M soln. in hexane) added to soln. of TMTH (1.50 mmol) in hexane under Ar, stirred for 3 h at room temp., 1-bromoheptane (1.50 mmol) added, heated to reflux for 2 h; analyzed by GC;
n-butyllithium in hexane 1-iodoheptane (1 equiv.) and TMTH (1 equiv.) in hexane cooled to 0°C under Ar, n-BuLi (1 equiv., 2.40 M in hexane) added, stirred for 15 min, quenched with water; analyzed by GC;
n-butyllithium in hexane 2-bromoheptane (1 equiv.) and TMTH (1 equiv.) in hexane cooled to 0°C under Ar, n-BuLi (1 equiv., 2.40 M in hexane) added, stirred for 5 min, quenched with water; analyzed by GC;
in hexane; cyclohexane to soln. of 1-iodoheptane (1.0 mmol) and TMTH (1.0 mmol) in hexane at 0°C added LDA (1.0 mmol, 1.6 M soln. in cyclohexane) under Ar, react. time 10 min; analyzed by GLPC;
