in neat (no solvent)
under N2; Al-compd. added slowly over a period of 2 h to Sb-compd. at 0°C with stirring, warmed slowly to room temp., stirred for 4 h, heated for 12 h at 120°C;; monitored by NMR, fractional distn., Al-compd. isolated by distn.;;
参考文献
Thomas, C. J.; Krannich, L. K.; Watkins, C. L.
Polyhedron, 1993 , vol. 12, p. 89 - 94
in tetrahydrofuran
(Ar); soln. of Sb compd. and Mg turnings was stirred for 3 h at room temp.; THF was removed in vac. and residue sepd. by distn.; elem. anal.; Bu3Sb was identified by MAS and b. p.;
参考文献
Breunig, Hans Joachim; Kanig, Walter
Journal of Organometallic Chemistry, 1980 , vol. 186, # 1 p. C5 - C8
chloro-trimethyl-silane; magnesium in tetrahydrofuran
(Ar), bromide droped to Mg-chips and Me3SiCl in THF, stirred for 12 h at 25°C; evapd. at reduced pressure, washed several times with pentane, solvent evapd., distilled at 60-80°C/0.01 mm Hg, detected by NMR,MS;
参考文献
Breunig, Hans Joachim; Severengiz, Tevfik
Zeitschrift fuer Naturforschung, Teil B: Anorganische Chemie, Organische Chemie, 1982 , vol. 37, # 4 p. 395 - 400
Nesmeyanov, A. N.; Borisov, A. E.; Novikova, N. V.; Fedin, E. I.; Petrovskii, P. V.
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1973 , p. 1776 - 1778
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1973 , p. 1833 - 1835