Treatment of K[Cp*Fe(CO)2]
(Cp*
=
η5-C5Me5) with ClSiMe2NR2
(R = Me, Et, iPr, Ph) in THF afforded Cp*(CO)2Fe(CH2)4OSiMe2NR2 accompanied with ring-opening and incorporation of a THF molecule between iron and silicon atoms. On the other hand, reactions between Li[Cp*Fe(CO)2] and ClSiMe2NR2 in diethyl ether (for R = Me, Et), or in toluene in the presence of N,N,Nâ²,Nâ²-tetramethylethylenediamine (TMEDA)
(for R =
iPr, Ph) afforded the corresponding Cp*(CO)2FeSiMe2NR2
(R = Me, Et, iPr, Ph), where the anionic complex was freshly prepared by treatment of Cp*(CO)2FeH with n-BuLi. In the case of the reaction of Li[Cp*Fe(CO)2] with ClSiMe2NPh2, although the formation of the diphenylamino derivative Cp*(CO)2FeSiMe2NPh2 was confirmed by NMR spectroscopy, purification of the product was unsuccessful. Subsequently, the exclusive formation of Cp*(CO)2FeSiMe2NPh2 was achieved by means of irradiation of Cp*(CO)2FeMe and HSiMe2NPh2 in toluene.
K[CP*Fe(CO)2]的处理
(CP*
=
η5-C5Me5) 与 ClSiMe2NR2
(R = Me, Et, iPr, Ph) 在 THF 中得到 CP*(CO)2Fe(
CH2)4OSiMe2NR2,同时开环并在
铁和
硅原子之间掺入 THF 分子。另一方面,Li[CP*Fe(CO)2] 和 ClSiMe2NR2 在
乙醚中(R = Me、Et)或在
甲苯中在 N,N,N-,N-2- 存在下发生反应
四甲基乙二胺 (TME
DA)
(对于 R =
iPr, Ph) 得到相应的 CP*(CO)2FeSiMe2NR2
(R = Me、Et、iPr、Ph),其中阴离子配合物是通过用 n-BuLi 处理 CP*(CO)2FeH 新鲜制备的。在Li[CP*Fe(CO)2]与ClSiMe2NPh2反应的情况下,虽然通过NMR光谱证实了二苯
氨基衍
生物CP*(CO)2FeSiMe2NPh2的形成,但产物的纯化不成功。随后,通过在
甲苯中照射CP*(CO)2FeMe和HSiMe2NPh2,实现了CP*(CO)2FeSiMe2NPh2的排他形成。