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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(yīng)生成一種中性羰基氫化絡(luò)合物[RuII(MeQ)(PPh3)2(CO)(H)](1)。在相似的反應(yīng)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(yīng)膦配體的目標(biāo)羰基氫化絡(luò)合物RuII(MeQ){P(C6H4Me)3}2(CO)(H)] (2) 和 [RuII(MeQ){P(C6H4OMe)3}2(CO)(H)] (3)。 這些絡(luò)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(luò)合物 [RuII(PPh3)3(Cl)2]和甲醇在堿性條件下反應(yīng)生成羰基氫化絡(luò)合物[RuII(PPh3)3(CO)(Cl)(H)]，11在其它過渡金屬絡(luò)合物中經(jīng)常有報(bào)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(luò)合物的生成反應(yīng)中的作用，[RuII(PPh3)3Cl2]和 MeQH 間的反應(yīng)也在乙醇中進(jìn)行了試驗(yàn)。主要的反應(yīng)產(chǎn)物經(jīng)表征為羰基甲基絡(luò)合物[RuII(MeQ)(PPh3)2(CO)(CH3)] (4)，此絡(luò)合物在空氣中穩(wěn)定，具有反磁性。 這一反應(yīng)與通過[(Tp)RuIICl(PPh3)(CH3CN)] 和NaBH4 在乙醇中生成相應(yīng)的羰基甲基絡(luò)合物[TpRuII(CH3)(CO)(PPh3)] 的反應(yīng)相似。當(dāng)[RuII(PPh3)3Cl2] 和 MeQH 的反應(yīng)在nPrOH （正丁醇）中進(jìn)行時(shí)，也生成了乙基羰基絡(luò)合物[RuII(MeQ)(PPh3)2(CO)(CH2CH3)]。然而，此乙基羰基絡(luò)合物在溶液中不穩(wěn)定，推測(cè)可能是由于Ru-CH2CH3的自發(fā)β-H 消除形成了烯烴絡(luò)合物。反過來說，當(dāng)反應(yīng)在苯甲醇中進(jìn)行時(shí)，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
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3樓2012-05-15 09:24:21
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