双(五甲基环戊二烯)钌(II)合成路线 (共 15 条)
反应条件
lithium carbonate in water; isopropyl alcohol T=90°C; 4 h; Inert atmosphere;
参考文献
UMICOR AG and CO. KG
Patent: WO2009/146870 A1, 2009 ;
Location in patent: Page/Page column 14 ;
反应条件
lithium carbonate in water; isopropyl alcohol T=90°C; 4 h;
参考文献
UMICORE AG and Co. KG
Patent: US2011/184203 A1, 2011 ;
Location in patent: Page/Page column 5 ;
反应条件
methyl iodide in tetrahydrofuran treatment of the starting complex with MeLi at -78°C in THF, stirred for 1 h, addn. of CH3I;
参考文献
Journal of the American Chemical Society, , vol. 116, # 14 p. 6468 - 6469
反应条件
in ethanol (N2); RuCl3 and ligand in EtOH were refluxed for 3 h, on cooling to room temp. pptd. brown solid; pptn. filtered out, washed with EtOH, ether and pentane, drying in vac. yielded main product; chromy. of the vol. reduced washings (alumina, ether) and removal of solvents afforded decamethylruthenocene;
参考文献
Journal of the American Chemical Society, , vol. 110, p. 6130
反应条件
Li2CO3 in ethanol; acetonitrile soln. of Ru-complex and 10 equiv. of Li2CO3 in a mixt. of ethanol, 1.25 equiv. of MeCN and ligand were refluxed for 4 h under N2; solvent was evapd., residue was extd. with Et2O and filtered over alumina, soln. was cooled to -80 °C, elem. anal.;
参考文献
Bauer, Andre
Organometallics, 2000 , vol. 19, # 25 p. 5471 - 5476
反应条件
in ethanol inert atmosphere; refluxing (1.5 h); filtration, cooling to 0°C (pptn.), filtration, washing (cold EtOH, Et2O); elem. anal.;
参考文献
Liles, David C.; Shaver, Alan; Singleton, Eric; Wiege, Manfred B.
Journal of Organometallic Chemistry, 1985 , vol. 288, p. C33 - C36
反应条件
NaBH4 in ethanol; water soln. of NaBH4 in 50percent aq. EtOH was added dropwise to a soln. of C5Me5H and RuCl3 in 90percent EtOH at 45°C, mixt. was stirred for 5 h at 45°C; filtered, residue was washed with benzene, combined org. exts. were evapd., residue was dissolved in acetone, cooled, ppt. was recrystd. from acetone;
参考文献
Kreindlin, A. Z.; Petrovskii, P. V.; Rybinskaya, M. I.; Yanovskii, A. I.; Struchkov, Yu. T.
Journal of Organometallic Chemistry, 1987 , vol. 319, p. 229 - 238
反应条件
zinc in ethanol under inert atm. soln. Ru complex and Zn dust in EtOH were stirred at room temp. for 5 min, 4-trimethylsiloxy-3-penten-2-one was added and stirred for 22 h; ppt. was filtered, dissolved in toluene and concd., hexane was added, recrystn. from CH2Cl2-hexane at -78°C - (Cp*Ru(C6H5Me))Cl, filtratewas evapd., extd. with toluene and chromed. on alumina - (Ru(acac)3);
参考文献
Organometallics, , vol. 27, # 23 p. 6071 - 6082
反应条件
Co(C5H5)2Cl in dichloromethane-d2 to soln. of Ru complex in CD2Cl2 added CoCp2Cl; monitored by NMR, pptd. by addn. of Et2O;
参考文献
Journal of Organometallic Chemistry, , vol. 289, p. 133 - 140
反应条件
in hexane under strict exclusion of air and moisture using vac. line and glove boxtechniques and Schlenk glassware; Ga complex (12 equiv.) added dropwise to suspn. of Ru complex in n-hexane at room temp.; filtered; washed (n-hexane); dried; redissolved in toluene; filtered; solvent removed (vac.); recrystd. (n-hexane); elem anal.;
参考文献
Cokoja, Mirza; Gemel, Christian; Steinke, Tobias; Schroeder, Felicitas; Fischer, Roland A.
Dalton Transactions, 2005 , # 1 p. 44 - 54