三(2,2,6,6-四甲基-3,5-庚二酮酸)钌(III)合成路线 (共 5 条)
反应条件
potassium hydrogencarbonate in ethanol; water RuCl3 in EtOH and water was refluxed for 4-5 h. An excess amount of theligand was added to the blue soln. and the mixture was refluxed until its color turned red. After cooling KHCO3 was added in several portions, followed always by 1-3 h reflux.; concn., filtration, extn.(benzene),The extn. was chromd., evapn. ,recrystn. (EtOH);
参考文献
Endo, Akira; Shimizu, Kunio; Sato, Gen P.; Mukaida, Masao
Chemistry Letters, 1984 , p. 437 - 440
反应条件
H2O2 in ethanol; water hydrated RuCl3 was refluxed in H2O/EtOH for 4-5 h; excess amount of ligand was added; mixture refluxed (0.5 - 2-3 h); cooled; KHCO3 added to neutralize H(1+); mixture refluxed for 1-2 h; procedure repeated; refluxed 1-3 h; H2O2 added dropwise; concd., ppt. filtered off, dried under a vacuum; ppt. extd. with benzene, passed through Al2O3, column washed with benzene, evapd. to dryness, recrystd. from EtOH;;
参考文献
Endo, Akira; Kajitani, Masatsugu; Mukaida, Masao; Shimizu, Kunio; Sato, Gen P.
Inorganica Chimica Acta, 1988 , vol. 150, p. 25 - 34
反应条件
sodium hydrogencarbonate in neat (no solvent) educts and NaHCO3 refluxed at 160°C for 6 h, addnl. NaHCO3 added, reflux continued at 210°C for 18 h; evapd. in vac., extd. into CCl4, evapd., dissolved in benzene, passed through column of Al2O3 (activity II-III), concd., pptd. by adding MeCN and water, crystals collected by filtration, dried in vac.; elem. anal.;
参考文献
Lashdaf; Hatanpaeae; Tiitta
Journal of Thermal Analysis and Calorimetry, 2001 , vol. 64, # 3 p. 1171 - 1182
反应条件
KOH in water prepn. according to N. B. Morozova et al., Coord. Chem., 1989, 15, 110 by reduction RuF6(1-) in acidic media and interaction of aqua-complexes of Ru(3+) with β-diketone at heating and neutralization with KOH up to pH 5-6; purified by vac. zone sublimation at pressure of 6 Pa and temp. 323-473 K; identified by mass spectrometry;
参考文献
Morozova; Zherikova; Semyannikov; Trubin; Igumenov
Journal of Thermal Analysis and Calorimetry, 2009 , vol. 98, # 2 p. 395 - 399
反应条件
hydrogen H2 atmosphere; thermogravimetry; x-ray powder diffraction anal.;
参考文献
Sov. J. Coord. Chem. (Engl. Transl.), , vol. 15, p. 67 - 72
Koordinatsionnaya Khimiya, , vol. 15, p. 110 - 115