二(五甲基环戊二烯基)六氟磷酸钴(III)合成路线 (共 8 条)
反应条件
t-BuLi in tetrahydrofuran C5Me5H in THF was treated with hexane soln. of t-BuLi at -78°C; warming to room temp; addn. of CoCl2 (Ar); stirring at room temp. for 12h; treating with NH4PF6; stirring at room temp. for 12 h; filtration, washing with THF and water, drying in vac., extn. into acetone, filtration, concn., pptn. with hexane, washing with hexane, drying in air, crystn. from acetone; elem. anal.;
参考文献
Robbins,J.L.; Edelstein,N.; Spencer,B.
Journal of the American Chemical Society, 1982 , vol. 104, p. 1882
反应条件
tert.-butyl lithium; iron(III) chloride in tetrahydrofuran; hydrogenchloride; hexane t-BuLi added to Me5C5 THF soln. by stirring at -70°C, warmed slowly to room temp., after 4 h CoBr2*1,2-dimethoxyethane added and boilingfor 12 h, cooled, added FeCl3 in aq. HCl, solvents evacuated; H2O added, extd. with ether, filtered, NH4PF6 adding, elem.anal.;
参考文献
Koelle, Ulrich; Khouzami, Fouad
Chemische Berichte, 1981 , vol. 114, # 9 p. 2929 - 2937
反应条件
iron(III) chloride in tetrahydrofuran; diethyl ether; water LiC5Me5 and Co-compound refluxed in THF/ether for 12 h, oxydized in situ with FeCl3; pptd. as PF6-salt from water;
参考文献
Koelle, Ulrich; Khouzami, Fouad
Angewandte Chemie, 1980 , vol. 92, p. 658 - 659
反应条件
oxygen in dichloromethane not isolated;
参考文献
Chemical Communications, , # 33 p. 3467 - 3469
反应条件
Na#Hg in tetrahydrofuran stirring for 12 h; decantation, evapn., sublimation in vac., crystn. from hexane; elem. anal.;
参考文献
Robbins,J.L.; Edelstein,N.; Spencer,B.
Journal of the American Chemical Society, 1982 , vol. 104, p. 1882
反应条件
in tetrahydrofuran stirring (20°C, 2 h); evapn., extn. (water, Et2O);
参考文献
Maryin; Petrovskii; Krasilmkova
Russian Chemical Bulletin, 1996 , vol. 45, # 10 p. 2427 - 2430
反应条件
in tetrahydrofuran stirring (20°C, 2 h); evapn., extn. (hexane), chromy. (Al2O3, hexane); elem. anal.;
参考文献
Maryin; Petrovskii; Krasilmkova
Russian Chemical Bulletin, 1996 , vol. 45, # 10 p. 2427 - 2430
反应条件
in tetrahydrofuran stirring (20°C, 2 h); evapn., extn. (water, Et2O), chromy. (Al2O3, hexane), recrystn. (toluene/hexane); elem. anal.;
参考文献
Maryin; Petrovskii; Krasilmkova
Russian Chemical Bulletin, 1996 , vol. 45, # 10 p. 2427 - 2430