Organometallic chemistry in a conventional microwave oven: the facile synthesis of group 6 carbonyl complexes
作者:Michael Ardon、Graeme Hogarth、Daniel T.W Oscroft
DOI:10.1016/j.jorganchem.2004.04.030
日期:2004.8
however, this reaction requires an inert atmosphere. While W(CO)6 reacts rapidly with amines to give cis diamine adducts in high yields, direct reactions with phosphines are not so clean. Bis(phosphine) complexes are, however, cleanly formed when a small amount of piperidine is added to the reaction mixture, presumably via the bis(piperidine) complex cis-[W(CO)4(pip)2]. Reactions with Cr(CO)6 generally
通过在改进的常规微波炉中进行反应,可以改善,加速和简化通过回流进行的合成。为了证明这种方法的潜力,据报道合成了20多种第6组有机金属化合物。六羰基,最著名的是Mo(CO)6,在改良的常规微波炉中与一定范围的单,双和三齿配体反应。它们通常在没有惰性气氛的情况下进行,产率高且反应时间短。例如,在20分钟内以大于95%的收率制备顺式[[Mo(CO)4(dppe)]。Mo(CO)6与二环戊二烯的反应可简单地一步合成[CpMo(CO)3 ]。2个在> 90%的产率,这与在甲苯中的炔烃以产生dimetallatetrahedrane衍生物进一步反应,混合[Cp 2沫2(CO)4(μ-RC 2 R)]; 大概是通过原位形成对空气敏感的[CpMo(CO)2 ] 2来实现的。还可以在45分钟内以48%的收率制备四乙酸二钼酸乙酯,但是,该反应需要惰性气氛。W(CO)6与胺快速反应以高产率生成顺式二胺加合物,但