氯化三(三苯基膦)合铑(I)合成路线 (共 95 条)
反应条件
trimethylamine oxide dihydrate in acetonitrile byproducts: trimethylamine, CO2; soln. of Rh-complex and Me3NO*2H2O in CH3CN boiled under reflux (1 h), mixt. cooled, evapn. of solvent (vac.), addn. of Ph3P and isopropanol to oily residue, react. mass boiled (1 h); cryst. ppt. filtered, washed (1. EtOH, 2. Et2O), dried (air);
参考文献
Kukushkin, V. Yu.; Dushina, M. E.; Krylov, V. K.; Iretskii, A. V.
Sov. J. Coord. Chem. (Engl. Transl.), 1987 , vol. 13, p. 364 - 369
Koordinatsionnaya Khimiya, 1987 , vol. 13, p. 650 - 655
反应条件
in chlorobenzene under N2; Rh complex and chlorobenzene heated at 80°C (oil bath) for 1 h; detd. by (31)P NMR spectra;
参考文献
Journal of the American Chemical Society, , vol. 127, # 43 p. 15304 - 15321
参考文献
Journal of the American Chemical Society, , vol. 88, p. 4537 - 4538
Progr. Inorg. Chem., , vol. 28, p. 63 - 202
Journal of the Chemical Society [Section] A: Inorganic, Physical, Theoretical, , p. 1736 - 1740
反应条件
in acetone; benzene N2-atmosphere; dissoln. of stoich. amts. (benzene/acetone=1:1, 50°C), stirring (2 h); crystn. on cooling, filtration, washing (benzene/acetone=1:1), concn. offiltrate, crystn.; elem. anal.;
参考文献
Sacco, A.; Vasapollo, G.; Giannoccaro, P.
Inorganica Chimica Acta, 1979 , vol. 32, p. 171 - 174
反应条件
CO2; CH2Cl2 in benzene High Pressure; a soln. of ((C6H3)3P)3RhCH3 in C6H6 was pressurized with 70 psi of CO2 for 17 h; filtration; evapn. to dryness; dissolving in toluene; filtration; addn. of CH3OH; cooling to -78°C; dissolving of the crystals in CH2Cl2/CD2Cl2;; removal of solvent; dissolving in toluene; filtration; concg. of the filtrate and addn. of CH3OH; cooling at -11°C for 4 weeks; all manipulations were carried out under Ar;;
参考文献
Darensbourg, Donald J.; Groetsch, Georg; Wiegreffe, Philip; Rheingold, Arnold L.
Inorganic Chemistry, 1987 , vol. 26, p. 3827 - 3830
反应条件
tetra-n-butylammonium tetrafluoroborate in dichloromethane Kinetics; byproducts: i-Pr3C6H2O2SNC8H4(CH2OH)2(CH2NHSO2C6H2-i-Pr3)2; under Ar; stoich. amt. of Rh complex and HOCH2C2CH2OH reacted in CH2Cl2 contg. n-Bu4NBF4 in presence of PPh3 (excess) at 25°C; monitored by cyclic voltammetry;
参考文献
Organometallics, , vol. 28, # 20 p. 6036 - 6043
反应条件
tetra-n-butylammonium tetrafluoroborate in dichloromethane Kinetics; byproducts: i-Pr3C6H2O2SNC8H4(CH2OH)2(CH2N(BOC)SO2C6H2-i-Pr3)2; under Ar; stoich. amt. of Rh complex and HOCH2C2CH2OH reacted in CH2Cl2 contg. n-Bu4NBF4 in presence of PPh3 (excess) at 25°C; monitored by cyclic voltammetry;
参考文献
Organometallics, , vol. 28, # 20 p. 6036 - 6043
反应条件
hydrogenchloride; triphenylphosphine in ethanol byproducts: NH4Cl; according to Johnson, B. F. G., Segal, J. A., J. Chem. Soc., Dalton Trans., 1972, 1268; refluxing/stirring (15 min, CH2Cl2/MeOH 2:1 v/v, bubbling with HCl gas); concn. of mixt., pptn. on addn. of MeOH, CH2Cl2 and PPh3;
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , p. 1139 - 1142
反应条件
in not given byproducts: vinyl chloride, ethylene; under N2; Rh complex reacted with cis-1,2-dichloroethylene;
参考文献
Organometallics, , vol. 28, # 20 p. 5982 - 5991
反应条件
in benzene-d6 byproducts: ethylene, vinyl chloride, PPh3; under N2; Rh complex and cis-1,2-dichloroethylene mixed in C6D6 at room temp.; detd. by (31)P NMR spectra;
参考文献
Organometallics, , vol. 28, # 20 p. 5982 - 5991