in neat (no solvent)
Iron atoms were codeposited with toluene at -196°C over 30 min, the mixt. was warmed to -78°C and cyclopentadiene was distilled into the reactor, the mixt. was warmed to room temp.;; filtered, evapd., ferrocene was removed by fractional sublimation, three isomers were inseparable;;
参考文献
Beard, Loren K.; Silvon, Michael P.; Skell, Philip S.
Journal of Organometallic Chemistry, 1981 , vol. 209, # 2 p. 245 - 254
in tetrahydrofuran
N2-atmosphere; addn. of equimolar mixt. of ligands to FeCl2 (-78°C), slow warming to room temp., stirring for 1 h; solvent removal (vac.), extn. into hexane, filtration, solvent removal (vac.), chromy. (Al2O3, 2percent THF in hexane);
参考文献
Dong, Teng-Yuan; Chang, Chung-Kay; Cheng, Ching-Hung
Journal of Organometallic Chemistry, 1999 , vol. 587, # 1 p. 46 - 48
in dichloromethane
(Ar); soln. of Ru complex and Fe complex in CH2Cl2 was refluxed for 3 h; solvent removed; chromd. (silica gel, CH2Cl2 or CH2Cl2/EtOAc); recrystd.(Et2O/hexane); elem. anal.;
参考文献
Katayama, Taku; Onitsuka, Kiyotaka; Takahashi, Shigetoshi
Journal of Organometallic Chemistry, 2006 , vol. 691, # 10 p. 2245 - 2256
in hexane; deuterated toluene; toluene
1 equiv. of Me2AlCl in 1.0 M hexane soln. was added to toluene soln. of Fe-compd. at -78 °C, stirring at this temp. for 1 h and at room temp. for 20 h, Me2AlCl was added dropwise in toluene-d8 at -50 °C; soln. was centrifuged, volatiles were removed in vac., detected by (13)CNMR;
参考文献
Wrackmeyer, Bernd; Klimkina, Elena V.; Ackermann, Tamara; Milius, Wolfgang
Inorganic Chemistry Communications, 2007 , vol. 10, # 7 p. 743 - 747
in toluene
1 equiv. of pyridine was added to a mixt. of Fe-compds. in toluene at -70 °C, stirring at room tmep. for 20 h; soln. was centrifuged, volatiles were removed in vac., some unidentifiedother compds. were also formed ((1)H and (13)C NMR);
参考文献
Wrackmeyer, Bernd; Klimkina, Elena V.; Ackermann, Tamara; Milius, Wolfgang
Inorganic Chemistry Communications, 2007 , vol. 10, # 7 p. 743 - 747
in deuterated toluene
(strict exclusion of air and moisture), mixt. of Al complexes (4:1) dissolved in toluene-d8 in NMR tube, heated at 120°C for 12 h; crystd. for 1 d;
参考文献
Wrackmeyer, Bernd; Klimkina, Elena V.; Milius, Wolfgang
European Journal of Inorganic Chemistry, 2009 , # 21 p. 3155 - 3162
in diethylamine
addn. of C5H6 to Fe(2+) halogenide at ambient temp. and presence of high excess of NH(C2H5)2;;
参考文献
Gelius, R.; Uhlmann, W.; Sperling, W.
Z. Chem. (Leipzig), 1966 , vol. 6, p. 227 - 228
Full Text Show Details
Gmelin Handbook: Fe: Org.Verb.A1, 2.1.1.2, page 16 - 18