n-butyllithium in diethyl ether; hexane Addn. of butyl-lithium in hexane to a soln. of the alkyne in anhyd. ether at -30°C, stirring for 15 min under dry N2, addn. of a soln. of the trialkylchlorostannane in ether, stirring for 30 min, rising temp. to room temp. during 1h.; Addn. of light petroleum, filtration under a stream of dry N2, evapn., distn. at reduced pressure.;
参考文献
Moloney, Mark G.; Pinhey, John T.; Roche, Eric G.
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry, 1989 , p. 333 - 342
in tetrahydrofuran under N2, addn. of Li-compd. in THF over 30 min at 0°C to Me3SnCl in THF, stirred for 18 h; removal of solvent, residue washed with water, extd. (ether), recrystd. (hexane);
参考文献
Dallaire; Brook; Bain; Frampton; Britten
Canadian Journal of Chemistry, 1993 , vol. 71, # 10 p. 1676 - 1683
Becerra, Rosa; Boganov, Sergey E.; Egorov, Mikhail P.; Faustov, Valery I.; Krylova, Irina V.; Nefedov, Oleg M.; Walsh, Robin
Journal of the American Chemical Society, 2002 , vol. 124, # 25 p. 7555 - 7562
n-butyllithium byproducts: Sn; (Ar); for 2.5 h at 200°C; dissolution in C6D6; filtration; addn. of n-BuLi; hydrolysis with ice water; drying of organic phase (MgSO4); fractionation;
参考文献
Appler, Hubertus; Neumann, Wilhelm P.
Journal of Organometallic Chemistry, 1986 , vol. 314, p. 247 - 260
in methanol a mixt. of Me3GeSnMe3 and Me3SnCl in methanol was kept for 30 h, reaction was followed by (1)H NMR spectroscopy; reaction was 91percent complete; not isolated, identified by (1)H NMR spectrum, polymer was isolated from a separate expt. and identified by mass spectrum;
参考文献
Cuthberston, Matthew J.; Wells, Peter R.
Journal of Organometallic Chemistry, 1985 , vol. 287, p. 25 - 38
in methanol-d4 a mixt. of Me3GeSnMe3 and Me3SnCl in CD3OD was kept for 30 h, reaction was followed by (1)H NMR spectroscopy; not isolated, identified by (1)H NMR spectrum;
参考文献
Cuthberston, Matthew J.; Wells, Peter R.
Journal of Organometallic Chemistry, 1985 , vol. 287, p. 25 - 38
n-butyllithium in tetrahydrofuran; diethyl ether; hexane under N2, n-BuLi in hexane cooled to -78°C, dild. with Et2O, ethereal soln. of heterocycle added dropwise with stirring, stirred for a while, after addn. of soln. of Me3SnCl in THF allowed to warm to room temp.; concd. in vac., methylcyclohexane added, filtered, fractionally distd.;elem. anal.;
参考文献
Jutzi, Peter; Gilge, Ullrich
Journal of Organometallic Chemistry, 1983 , vol. 246, # 2 p. 163 - 168
