反式-双(三苯基膦)合氯化羰基铑(Ⅰ)合成路线 （共 95 条）
反应条件
chloroform at room temp. during 16 h under CO;
参考文献
Booth, Brian L.; Casey, Geoffrey C.; Haszeldine, Robert N.
Journal of Organometallic Chemistry, 1981 , vol. 219, # 3 p. 401 - 408
反应条件
in further solvent(s) argon-filled glovebox, durene, bibenzyl, 130°C, 23h; product detd. by GC and IR;
参考文献
Organometallics, , vol. 8, p. 2703 - 2708
反应条件
in solid byproducts: triphenylphosphine oxide, CO, O2; thermal decompn. (in air or helium stream, 3-4 h, 160°C); sepn. of Rh(phen)2ClO4 (extn., EtOH; IR spectroscopy), extn. of OPPh3 (ether), sepn. of Rh(CO)(PPh3)2 (extn., CHCl3); DTA monitoring, elem. anal.;
参考文献
Kukushkin, Yu. N.; Iretskii, A. V.; Danilina, L.I.; Abdurakhmanov, R. O.
Russian Journal of Inorganic Chemistry (Translation of Zhurnal Neorganicheskoi Khimii), 1986 , vol. 31, p. 233 - 236
Zhurnal Neorganicheskoi Khimii, 1986 , vol. 31, p. 413 - 416
反应条件
in solid byproducts: triphenylphosphine oxide, CO, O2; thermal decompn. (in air or helium stream, 3-4 h, 160°C); sepn. of Rh(bipy)2ClO4 (extn., EtOH; IR spectroscopy), extn. of OPPh3 (ether), sepn. of Rh(CO)(PPh3)2 (extn., CHCl3); DTA monitoring, elem. anal.;
参考文献
Kukushkin, Yu. N.; Iretskii, A. V.; Danilina, L.I.; Abdurakhmanov, R. O.
Russian Journal of Inorganic Chemistry (Translation of Zhurnal Neorganicheskoi Khimii), 1986 , vol. 31, p. 233 - 236
Zhurnal Neorganicheskoi Khimii, 1986 , vol. 31, p. 413 - 416
反应条件
in dichloromethane FpCH2COFp and RhCl(PPh3)3 are dissolved in CH2Cl2 (Ar), stirring (6h, room temp.).; Filtration of RhCl(PPh3)2(CO), chromy. of filtrate, elem. anal.;
参考文献
Organometallics, , vol. 7, p. 366 - 374
反应条件
in tetrahydrofuran a soln. of Ph2CCl2 in THF was added under N2 to a suspn. of Rh-complex in the same solvent in 1:1 mole ratio, mixt. was stirred at 50°C for 3.5 h; solvent was removed, residue chromd. over Al2O3 (eluent hexane for Ph2C=CPh2 and CHCl3 for RhCl(CO)(PPh3)2);
参考文献
Journal of Organometallic Chemistry, , vol. 224, # 2 p. 197 - 205
反应条件
sodium amalgam in tetrahydrofuran Rh complex treated with sodium amalgam in THF at room temp. for 3 h, excess of amalgam filtered, soln. added under CO atmosphere to soln. of org. compd. over 45 min, mixture stirred at room temp. for 2 d; filtration, concn., addn. of light petroleum, filtration, addn. of MeOH, washing (light petroleum), drying in vac.; elem. anal.;
参考文献
Booth, Brian L.; Casey, Sylvia; Haszeldine, Robert N.
Journal of Organometallic Chemistry, 1982 , vol. 226, # 3 p. 289 - 300
反应条件
in tetrahydrofuran a suspn. of Rh complex and Ph2CClCClPh2 in THF in 1:1 mole ratio was heated at 50°C for 3.5 h under N2; evapd., residue extd. with EtOH (ext. contained Ph2C=CPh2), with THF togive a solid ext., which was recrystd. from CHCl3/hexane to give RhCl3(CO)(PPh3)2 which was filtered off, filtrate was evapd., residue crystd. from C6H6/MeOH to give RhCl(CO)(PPh3)2;
参考文献
Journal of Organometallic Chemistry, , vol. 224, # 2 p. 197 - 205
反应条件
in tetrahydrofuran byproducts: carbon monoxide; mixture was stirred at room temp. for 15 h under CO; chromd. (alumina), recrystd. from CHCl3/EtOH;
参考文献
Booth, Brian L.; Casey, Geoffrey C.; Haszeldine, Robert N.
Journal of Organometallic Chemistry, 1981 , vol. 219, # 3 p. 401 - 408
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
