n-butyllithium in tetrahydrofuran under Ar or N2, Schlenk technique; soln. of n-BuLi (1 equiv.) added dropwise to soln. of Fe compd. at -60°C, mixt. stirred at room temp. for 0.5 h, cooled to -30°C, P compd. (1 equiv.) added dropwise, mixt. stirred at room temp. for 1 h; concn. under vac., chromy. (n-hexane), dried under vac.;
参考文献
Milde, Bianca; Lohan, Manja; Schreiner, Claus; Rueffer, Tobias; Lang, Heinrich
European Journal of Inorganic Chemistry, 2011 , # 35 p. 5437 - 5449
triethylamine in tetrahydrofuran under Ar; soln. of iodoferrocene (0.5 mmol), PdCl2(PPh3)2 (0.025 or 0.05mmol), CuI (0.01 or 0.02 mmol) dissolved in THF, triethylamine (1 mmol) , and alkyne (0.5 or 1.25 mmol) added, atm. changed for CO, heated at 60°C for 12 h; solvent removed in vacuo, column chromy. (silica gel, toluene); elem. anal.;
caesium carbonate in tetrahydrofuran under Ar; soln. of iodoferrocene (0.5 mmol), PdCl2(PPh3)2 (0.025 or 0.05mmol), CuI (0.01 or 0.02 mmol) dissolved in THF, Cs2CO3, and alkyne (0. 5 or 1.25 mmol) added, atm. changed for CO, heated at 60°C for 32h; solvent removed in vacuo, column chromy. (silica gel, toluene); elem. anal.;
triethylamine in tetrahydrofuran
under Ar; soln. of iodoferrocene (0.5 mmol), PdCl2(PPh3)2 (0.025 or 0.05mmol), CuI (0.01 or 0.02 mmol) dissolved in THF, triethylamine (1 mmol) , and alkyne (0.5 or 1.25 mmol) added, atm. changed for CO, heated at 60°C for 12 h; solvent removed in vacuo, column chromy. (silica gel, toluene); elem. anal.;
Sato, M.; Ito, T.; Motoyama, I.; Watanabe, K.; Hata, K.
Bulletin of the Chemical Society of Japan, 1969 , vol. 42, p. 1976 - 1981
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Gmelin Handbook: Fe: Org.Verb.A1, 5.1.2.1.2, page 366 - 368
