三羰基五甲基环戊二烯基铼合成路线 （共 27 条）
反应条件
in neat (no solvent)
byproducts: CO; stirred at 150°C for 0.5 h, heated to 210°C over 2-5 h, kept at 210°C for 0.5 h, N2 atm.; cooling, washing with cold hexane, drying with a stream of air;
参考文献
Patton,A.T.; Strouse,C.E.; Knobler,C.B.
Journal of the American Chemical Society, 1983 , vol. 105, p. 5804
反应条件
(CH3)5C5ReH6 in hexane
stirring (room temp., 15 min), evapn. (vac.); extg. (hexane), concg., crystn. (-40°C); detd. by NMR spectroscopy;
参考文献
Ghosh, Sundargopal; Shang, Maoyu; Fehlner, Thomas P.
Journal of the American Chemical Society, 1999 , vol. 121, # 32 p. 7451 - 7452
反应条件
in hexane
byproducts: H2, CO; (Ar); for 15 min; evapd., extd. (hexane), ext. concd., crystd. at -40°C fractionally, mother liquor concd., chromd. (SiO2), concd., crystd. at -40°C overnight, crystals sepd. manually, recrystd. at -4°C; obtainedanal. impure;
参考文献
Ghosh; Lei; Shang; Fehlner
Inorganic Chemistry, 2000 , vol. 39, # 23 p. 5373 - 5382
反应条件
H2O2; H2SO4 in water; benzene
React. of Re-compd. with aq. H2O2 (30percent) in a 2-phase benzene/water system, addn. of H2SO4 after 3 h and prompt termination of react.; Washing of org. phase with NaHCO3 soln., drying with MgSO4 and removal of solvent. Recrystn. from toluene/pentane.;
参考文献
Paciello, Rocco A.; Kiprof, Paul; Herdtweck, Eberhardt; Herrmann, Wolfgang A.
Inorganic Chemistry, 1989 , vol. 28, p. 2890 - 2893
反应条件
trifluoroacetic acid in tetrahydrofuran
参考文献
Zobi, Fabio; Spingler, Bernhard; Alberto, Roger
European Journal of Inorganic Chemistry, 2008 , # 27 p. 4205 - 4214
反应条件
in tetrahydrofuran; diethyl ether
N2-atmosphere; mixing MeLi (in Et2O) with slight excess of Cu-compd. (inTHF) at -23°C, addn. of 0.33 equiv. of Re-complex, stirring (-23 °C, 30 min, then room temp., 45 min); concn. (vac.), addn. of H2O, filtration (Celite), solvent removal, chromy. (SiO2, hexane); elem. anal.;
参考文献
Klahn, A. Hugo; Manzur, Carolina; Toro, Adriana; Moore, Madeleine
Journal of Organometallic Chemistry, 1996 , vol. 516, # 1-2 p. 51 - 57
反应条件
in dichloromethane
standard Schlenk techniques; Re-compd. dissolved in CH2Cl2 at room temp.under N2, stirred for 5 h with C6H5NH2; solvent pumped off, crystallized from hexane-CH2Cl2, elem. anal.;
参考文献
Aballay, Alvaro; Buono-Core, Gonzalo E.; Godoy, Fernando; Klahn, A. Hugo; Ibanez, Andres; Garland, Maria Teresa
Journal of Organometallic Chemistry, 2009 , vol. 694, # 23 p. 3749 - 3752
反应条件
in dichloromethane
standard Schlenk techniques; Re-compd. dissolved in CH2Cl2 at room temp.under N2, stirred for 5 h with CH3OC6H4NH2; solvent pumped off, crystallized from hexane-CH2Cl2, elem. anal.;
参考文献
Aballay, Alvaro; Buono-Core, Gonzalo E.; Godoy, Fernando; Klahn, A. Hugo; Ibanez, Andres; Garland, Maria Teresa
Journal of Organometallic Chemistry, 2009 , vol. 694, # 23 p. 3749 - 3752
反应条件
in benzene-d6
byproducts: C6H5OCH3, C6D5C6H4OCH3; (N2), ambient temp., overnight;
参考文献
Barrientos-Penna, Carlos F.; Gilchrist, Alan B.; Klahn-Oliva, A. Hugo; Hanlan, A. J. Lee; Sutton, Derek
Organometallics, 1985 , vol. 4, p. 478 - 485
反应条件
in hexane
byproducts: methane; Irradiation (UV/VIS); CO atmosphere, 1 atm; irradn. (200 W Hg lamp, room temp., 20 min);
参考文献
Leiva, Carmen; Klahn, A. Hugo; Godoy, Fernando; Toro, Adriana; Manriquez, Victor; Wittke, Oscar; Sutton, Derek
Organometallics, 1999 , vol. 18, # 3 p. 339 - 347
