三羰基(η-环戊二烯基)合锰合成路线 (共 55 条)
反应条件
in decalin T=200°C; 9 h; RefluxInert atmosphere;
参考文献
European Journal of Inorganic Chemistry, , # 36 p. 6018 - 6026
反应条件
in dichloromethane Electrolysis; controlled potential electrolysis at 0.5 V, CH2Cl2/0.05 M N(C4H9)4B(C6F5)4; electrochemical IR-spectra;
参考文献
Journal of the American Chemical Society, , vol. 130, # 30 p. 9859 - 9870
反应条件
P4 in tetrahydrofuran Ar atmosphere, addn. of Rh complex to soln. of Mn complex and P4, stirring (room temp., 10 min), concn. to dryness (70°C, vacuum); sublimation of CpMn(CO)3 and P4 (50°C, high vacuum), suspn. (n-pentane), filtration, extn. with hot filtrate, crystn.; elem. anal.;
参考文献
Chemische Berichte, , vol. 128, # 3 p. 251 - 258
反应条件
in dichloromethane under Ar atm. soln. CmNH2 in CH2Cl2 was treated with soln. acetic-formicanhydride in CH2Cl2 and stirred for 20 min; react. mixt. was washed with aq. Na2CO3 and water, dried over Na2SO4, concd. and chromed. on silica, solvent was removed in vacuo; elem. anal.;
参考文献
Organometallics, , vol. 23, # 12 p. 2927 - 2938
反应条件
in tetrahydrofuran; benzene byproducts: TlBr; Sonication; dark, N2 atmosphere; stirring (3 - 4 h); filtration, washing (C6H6), drying of org. extract, evapn., sublimation;elem. anal.;
参考文献
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, , vol. 27, # 9 p. 1299 - 1314
反应条件
N(CH2CH3)3 in tetrahydrofuran (N2); addn. of selenium compd. and amine to a soln. of iron carbonyl in THF, stirring at room temp. for 10 min, cooling to -100°C, pouring to manganese complex, warming to -80°C, stirring for 7-8 h at -80 to -45°C; evapn. at -50 to -40°C, column chromy (Al2O3, petroleum ether, petroleum ether/CH2Cl2 20:1, petroleum ether/CH2Cl2/Et2O 10:1:1), evapn., recrystn. (petroleum ether/CH2Cl2, -80°C); elem. anal.;
参考文献
Organometallics, , vol. 20, # 11 p. 2226 - 2233
反应条件
in toluene (N2, Schlenk technique); addn. of molybdenum compd. to THF soln. of manganese compd., dissolving in toluene, stirring at room temp. for 15 min; evapn., extn. (CH2Cl2/petroleum ether (1:7)), chromy. (alumina, CH2Cl2/petroleum ether 1:7, then 1:1) at 253 K, evapn., elem. anal.;
参考文献
Organometallics, , vol. 28, # 15 p. 4385 - 4393
反应条件
N(CH2CH3)3 in tetrahydrofuran (N2); addn. of selenium compd. and amine to a soln. of iron carbonyl in THF, stirring at room temp. for 10 min, cooling to -100°C, pouring to manganese complex, warming to -80°C, stirring for 7 h at -80to -50°C; evapn. at -50 to -40°C, column chromy (Al2O3, petroleum ether, petroleum ether/CH2Cl2 20:1, petroleum ether/CH2Cl2/Et2O 10:1:1), evapn., recrystn. (petroleum ether/CH2Cl2, -80°C); elem. anal.;
参考文献
Organometallics, , vol. 20, # 11 p. 2226 - 2233
反应条件
in hexane under Ar; addn. of P(O-i-Pr)3 hexane soln. to hexane soln. of complex, mixed 3h at 20°C; evapn., residue is dissolved in 1:1 hexane-diethyl ether mixt., chromd. (Al2O3), mixt. of CpMn(CO)3 and Cp(CO)2MnCCPhH, yellow band eluted with 1:1 hexane-methyl acetate, evapn. of solvent, oily residue treated with hexane/benzene, elem. anal.;
参考文献
Journal of General Chemistry USSR (English Translation), , vol. 57, p. 918 - 928
Zhurnal Obshchei Khimii, , vol. 57, p. 1030 - 1042
反应条件
in dichloromethane N2-atmosphere; refluxing (dark, 16.5 h); filtering, evapn., chromy. (alumina, Et2O), evapn., drying (vac.);
参考文献
Organometallics, , vol. 17, # 25 p. 5586 - 5590