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| Synthesis and Characterization. Reaction of [RuII(PPh3)3Cl2] with MeQH in the presence of Et3N in MeOH produces a neutral carbonyl hydrido complex [RuII(MeQ)(PPh3)2(CO)(H)] (1). Under similar reaction conditions using [RuII{P(C6H4Me)3}3Cl2] or [RuII{P(C6H4OMe)3}3Cl2] in place of [RuII(PPh3)3Cl2] also afforded the target carbonyl hydrido complexes with the corresponding phosphine ligands, [RuII(MeQ){P(C6H4Me)3}2(CO)(H)] (2) and [RuII(MeQ){P(C6H4OMe)3}2(CO)(H)] (3), respectively (Scheme 1a). The carbonyl and hydride ligands of these complexes are derived from the decarbonylation of primary alcohol (MeOH). Similar decarbonylation of methanol, such as the formation of carbonyl hydrido complex [RuII(PPh3)3(CO)(Cl)(H)] from the reaction between 16e– ruthenium complex [RuII(PPh3)3(Cl)2] and MeOH in the presence of base,11 are commonly reported in other transition metals complexes, in particular for those with 16e– Ru(II) metal center.[ (a) Bennet, M. A.; Bruce, M. I.; Matheson, T. W. In Comprehensive Organometallic Chemistry; Wilkinson, G.; Stone, F. G. A.; Abel, E. W.; Eds.; Pergamon Press: Oxford, U.K., 1982, Vol. 4, pp 721. (b) Chatt, J.; Shaw, B. L.; Field, A. E. J. Chem. Soc. 1964, 3466. (c) Benedetti, E.; Braca, G.; Sbrana, G.; Salvetti, F.; Grassi, B. J. Organomet. Chem. 1972, 37, 361. (d) Empsall, H. D.; Hyde, E. M.; Mentzer, E.; Shaw, B. L.; Uttley, M. F. J. Chem. Soc., Dalton Trans. 1976, 2069. (e) Chaudret, B. N.; Cole-Hamilton, D. J.; Nohr, R. S.; Wilkinson, G. J. Chem. Soc., Dalton Trans. 1977, 1546. (f) Cole- Hamilton, D. J.; Wilkinson, G. Nouv. J. Chim. 1977, 1, 142. (g) Gill, D. F.; Shaw, B. L. Inorg. Chim. Acta 1979, 33, 19. (h) Morton, D.; Cole-Hamilton, D. J.; Utuk, I. D.; Paneque-Sosa, M. J. Chem. Soc., Dalton Trans. 1989, 489. (i) Portnoy, M.; Frolow, F.; Milstein, D. Organometallics 1991, 10, 3960.] To elucidate the role of methanol in the formations of these carbonyl hydrido complexes, the reaction between the [RuII(PPh3)3Cl2] and MeQH was also carried out in ethanol. The major product was then characterized to be the carbonyl methyl complex [RuII(MeQ)(PPh3)2(CO)(CH3)] (4), which is an air-stable and diamagnetic. This reaction is similar to the formation of corresponding carbonyl methyl complex [TpRuII(CH3)(CO)(PPh3)] from the reaction of [(Tp)RuIICl(PPh3)(CH3CN)] (Tp = hydrotris(pyrazolyl)borate) with NaBH4 in EtOH.[ Chen, Y.-Z.; Chan, W. C.; Lau, C. P.; Chu, H. S.; Lee, H. L. Organometallics 1997, 16, 1241.] When the reaction of [RuII(PPh3)3Cl2] with MeQH was carried out in nPrOH, it also produces the ethyl carbonyl complex [RuII(MeQ)(PPh3)2(CO)(CH2CH3)]. However, the ethyl carbonyl complex is unstable in solution, presumably, due to spontaneous β-H elimination of Ru-CH2CH3 to form an alkene complex. On the other hand, when the reaction was carried out in PhCH2OH, it produced exclusively [RuII(MeQ)(PPh3)2(CO)(H)] (1) rather than [RuII(MeQ)(PPh3)2(CO)(Ph)]. |
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8814402
至尊木蟲 (職業(yè)作家)
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756762952: 金幣+30, 翻譯EPI+1, ★★★★★最佳答案 2012-05-15 10:13:23
756762952: 金幣+30, 翻譯EPI+1, ★★★★★最佳答案 2012-05-15 10:13:23
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合成和表征 [RuII(PPh3)3Cl2] 和 MeQH 在含有三乙胺的甲醇中反應生成一種中性羰基氫化絡合物[RuII(MeQ)(PPh3)2(CO)(H)](1)。在相似的反應條件下，用[RuII{P(C6H4Me)3}3Cl2] 或[RuII{P(C6H4OMe)3}3Cl2] 代替[RuII(PPh3)3Cl2] ，也分別得到具有相應膦配體的目標羰基氫化絡合物RuII(MeQ){P(C6H4Me)3}2(CO)(H)] (2) 和 [RuII(MeQ){P(C6H4OMe)3}2(CO)(H)] (3)。 這些絡合物的羰基和氫化物配體源自于伯醇（甲醇）的脫羧作用。 甲醇的相似的脫羧作用，諸如由16e–釕絡合物 [RuII(PPh3)3(Cl)2]和甲醇在堿性條件下反應生成羰基氫化絡合物[RuII(PPh3)3(CO)(Cl)(H)]，11在其它過渡金屬絡合物中經常有報道，尤其是那些具有16e– Ru(II) 金屬中心者為了闡明甲醇在這些羰基氫化絡合物的生成反應中的作用，[RuII(PPh3)3Cl2]和 MeQH 間的反應也在乙醇中進行了試驗。主要的反應產物經表征為羰基甲基絡合物[RuII(MeQ)(PPh3)2(CO)(CH3)] (4)，此絡合物在空氣中穩(wěn)定，具有反磁性。 這一反應與通過[(Tp)RuIICl(PPh3)(CH3CN)] 和NaBH4 在乙醇中生成相應的羰基甲基絡合物[TpRuII(CH3)(CO)(PPh3)] 的反應相似。當[RuII(PPh3)3Cl2] 和 MeQH 的反應在nPrOH （正丁醇）中進行時，也生成了乙基羰基絡合物[RuII(MeQ)(PPh3)2(CO)(CH2CH3)]。然而，此乙基羰基絡合物在溶液中不穩(wěn)定，推測可能是由于Ru-CH2CH3的自發(fā)β-H 消除形成了烯烴絡合物。反過來說，當反應在苯甲醇中進行時，專一性地生成[RuII(MeQ)(PPh3)2(CO)(H)] (1)，而非[RuII(MeQ)(PPh3)2(CO)(Ph)]. |
2樓2012-05-15 09:22:41
8814402
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