双(氯金(I))双(二苯基膦)甲烷合成路线 (共 12 条)
反应条件
in tetrahydrofuran under N2 atm. (ClAu)2dppm and TlBF4 were added to soln. (NEt4)2(Fe5MoC(CO)17) in THF and stirred at 0°C for 17 h; Et2O was added and mixt. was cooled for 2 h to -30°C, ppt. was filtered, filtrate was evapd. to dryness, residue was extd. with CH2Cl2, hexane was added at -30°C; elem. anal.;
参考文献
Reina, Roser; Rodriguez, Laura; Rossell, Oriol; Seco, Miquel; Font-Bardia, Merce; Solans, Xavier
Organometallics, 2001 , vol. 20, # 8 p. 1575 - 1579
反应条件
in ethanol; dichloromethane; chloroform
Au-complex in EtOH mixed with dppm in CH2Cl2, stirred for 30 min, CHCl3added, stirred for 1 h; set aside until the volume was reduced to 20 ml, filtered off, dried inair; elem. anal.;
参考文献
Lin, Ivan J. B.; Hwang, J. M.; Feng, Da-Fa; Cheng, M. C.; Wang, Yu
Inorganic Chemistry, 1994 , vol. 33, p. 3467 - 3472
反应条件
in not given
N2-atmosphere; stoich. amts.;
参考文献
Rossell, Oriol; Seco, Miquel; Segales, Gloria
Journal of Organometallic Chemistry, 1995 , vol. 503, # 2 p. 225 - 234
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Ferrer, Montserrat; Julia, Anna; Reina, Roser; Rossell, Oriol; Seco, Miquel; De Montauzon, Dominique
Journal of Organometallic Chemistry, 1998 , vol. 560, # 1-2 p. 147 - 153
反应条件
in methanol; dichloromethane
under N2; soln. of Au complex in MeOH added to soln. of ligand in CH2Cl2; stirred for 3 h; solvent removed in vac.; H2O added; filtered; ppt. washed with H2O and Et2O; dried in vac.;
参考文献
Sevillano, Paloma; Fuhr, Olaf; Hampe, Oliver; Lebedkin, Sergej; Matern, Eberhard; Fenske, Dieter; Kappes, Manfred M.
Inorganic Chemistry, 2007 , vol. 46, # 18 p. 7294 - 7298
反应条件
in acetone
addn. of soln. of dppm (1 equiv.) in acetone to suspn. of (AuCl(SMe)2) (2 equiv.) in acetone; stirring for 2 h; pptn., filtration, washing with acetone, diethyl ether and pentane, drying under vac.;
参考文献
Brandys, Marie-Claude; Jennings, Michael C.; Puddephatt, Richard J.
Journal of the Chemical Society, Dalton Transactions, 2000 , # 24 p. 4601 - 4606
反应条件
in dichloromethane
byproducts: [N(PPh3)2]ClO4; molar ratio Au2-dppm complex:AuCl2(1-) complex=1:2, stirring (room temp., 3 h); concn., pptn. on Et2O addn., washing (MeOH/Et2O=1:1);
参考文献
Bardaji, Manuel; Laguna, Antonio; Laguna, Mariano
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1995 , # 8 p. 1255 - 1258
反应条件
in water; acetone
addn. of thiodiglycol to NaAuCl4 in H2O/Me2CO, then addn. of phosphine (0.5 equiv.) in Me2CO (pptn.), stirring (30 min); filtration, washing (H2O), drying (vac.);
参考文献
Berners-Price, Susan; Sadler, Peter J.
Inorganic Chemistry, 1986 , vol. 25, p. 3822 - 3827
反应条件
in tetrahydrofuran
suspending Pd2(dppm)2Cl in THF, addn. of LiBF4 and stirring for 5 mins. addn. of Au(SEt2)Cl in THF (results in deep red soln.), stirring for 1 h, filtration; all manipulations under N2; redn. of volume, pptn. and washing with Et2O, removal of Au2(dppm)Cl2 by crystn. from THF, crystn. from CH2Cl2/pentane, fractional crystn.;
参考文献
Braunstein, Pierre; Luke, Michael A.; Tiripicchio, Antonio; Tiripicchio Camellini, Marisa
New Journal of Chemistry, 1988 , vol. 12, p. 429 - 434
反应条件
in dichloromethane
soln. of Pt-complex in CH2Cl2, addn. of Au-complex in CH2Cl2 (0°C), immediate color change from light to dark red, stirred (1 h); solvent removed (dark red solid), not isolated, monitored by NMR;
参考文献
Arsenault, G. J.; Puddephatt, R. J.
Canadian Journal of Chemistry, 1989 , vol. 67, p. 1800 - 1806
反应条件
in dichloromethane
soln. of Pt-complex in CH2Cl2, addn. of Au-complex in CH2Cl2 (0°C), immediate color change from orange to dark red, stirred (5 min, ambient temp.); solvent removed (dark red oil), not isolated, monitored by NMR;
参考文献
Arsenault, G. J.; Puddephatt, R. J.
Canadian Journal of Chemistry, 1989 , vol. 67, p. 1800 - 1806