(1,5-环辛二烯)氯铑(I)二聚体合成路线 (共 52 条)
反应条件
in acetonitrile byproducts: AgCl; addn. of AgBF4 to soln. of Rh-compd., pptn. of AgCl, stirring for 15 min.; filtration of pptd. AgCl, evapn.;
参考文献
Inorganica Chimica Acta, , vol. 160, p. 159 - 166
反应条件
lithium triethylborohydride in tetrahydrofuran slow addn. of THF soln. of LiB(C2H5)3H to soln. of Rh complex in THF cooled in ice bath, under dry N2; stirring at room temp. for 16 h;; removal of volatile components in vac.; extraction of residue with pentane; pentane extractant yields (RhH(C8H12))4; washing residue with THF; centrifugation yields Rh; heating in vac. at 400°C for 2 h; TEM; electron and X-ray diffraction;;
参考文献
Journal of Catalysis, , vol. 139, p. 504 - 512
反应条件
carbon monoxide; SnCl2; PPh3 in methanol; dichloromethane CO at atmosphere pressure was bubbled for 5 min through a CH2Cl2/MeOH soln. of Rh-complex, phosphine and SnCl2; product was obtained in low yield; CH2Cl2 was evapd., ppt. was collected;
参考文献
Garcia, V.; Garralda, M. A.; Zugasti, E.
Journal of Organometallic Chemistry, 1987 , vol. 322, p. 249 - 256
反应条件
triphenylphosphine in acetone byproducts: COD; N2-atmosphere; slow sequential addn. of stoich. amt. of dppe and seven-fold excess of PPh3 to Rh-complex (during 7 h); pptn. after 22 h;
参考文献
Sanger, Alan R.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1977 , p. 120 - 129
反应条件
in dichloromethane stoich. amts. of educts stirred for 2 h, concd. in vac., ether added, filtered; filtrate evapd. to dryness, residue pptd. with methanol/water; recrystd. from methanol/water;
参考文献
Uson, R.; Oro, L. A.; Ciriano, M. A.; Pinillos, M. T.; Cabeza, J. A.
Journal of Organometallic Chemistry, 1981 , vol. 221, # 2 p. 249 - 256
反应条件
in dichloromethane stoich. amts. of educts stirred for 2 h, concd. in vac., ether added, AuClPPh3 filtered; filtrate evapd. to dryness, residue pptd. with methanol/water; recrystd. from methanol/water;
参考文献
Uson, R.; Oro, L. A.; Ciriano, M. A.; Pinillos, M. T.; Cabeza, J. A.
Journal of Organometallic Chemistry, 1981 , vol. 221, # 2 p. 249 - 256
反应条件
P(C6H5)3 in THF-d8 (tetrahydrofuran-d8) addn. of 3 equiv. of PPh3 and catecholborane to soln. of Rh-complex (25°C, (11)B-NMR monitoring); not isolated;
参考文献
Burgess, Kevin; Van Der Donk, Wilfred A.; Westcott, Stephen A.; Marder, Todd B.; Baker, R. Thomas; Calabrese, Joseph C.
Journal of the American Chemical Society, 1992 , vol. 114, # 24 p. 9350 - 9359
反应条件
P(C6H5)3 in THF-d8 (tetrahydrofuran-d8) addn. of 2 or 3 equiv. of PPh3 to soln. of Rh-complex (25°C, NMR tube, addn. of catecholborane after 40 min), (31)P-NMR monitoring at -80°C; not isolated;
参考文献
Burgess, Kevin; Van Der Donk, Wilfred A.; Westcott, Stephen A.; Marder, Todd B.; Baker, R. Thomas; Calabrese, Joseph C.
Journal of the American Chemical Society, 1992 , vol. 114, # 24 p. 9350 - 9359
反应条件
in dichloromethane excess of AgSbF6, stirring for 1 h; volume reduction, pptn. on Et2O addn.;
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , # 21 p. 3069 - 3074
反应条件
in acetonitrile; benzene byproducts: AgCl, NaBF4; stirring (15 min), sepn. of AgCl (filtration off), addn. of ligand, stirring (overnight), evapn. of soln. to dryness, extn. (benzene), sepn. of NaBF4 (filtration off); removal of solvent, recrystn. (CH2Cl2/CH3CN);
参考文献
Rodman, Gary S.; Mann, Kent R.
Inorganic Chemistry, 1988 , vol. 27, p. 3338 - 3346