918148-11-5Relevant articles and documents
Amino-functionalised diarylphosphide complexes of the alkali metals and lanthanum
Izod, Keith,Liddle, Stephen T.,Clegg, William,Harrington, Ross W.
, p. 3431 - 3437 (2007/10/03)
The secondary phosphines Ar(C6H4-2-CH 2NMe2)PH [Ar = mes (3), Tripp (4)] may be isolated in good yields from reactions between Li(C6H4-2-CH 2NMe2) and the respective dichlorophosphine, followed by reduction with LiAlH4 [mes = 2,4,6-Me3C6H 2, Tripp = 2,4,6-Pri3C6H 2]. Metalation of either 3 or 4 with BunLi gives the corresponding lithium compound; the lithium derivative of 3 was isolated as the separated ion pair complex [Li(12-crown-4)2][(mes)(C 6H4-2-CH2NMe2)P]·THF (5). The lithium complexes Ar(C6H4-2-CH2NMe 2)PLi undergo metathesis reactions with either NaOBut or KOBut to give the heavier alkali metal phosphides {Ar(C 6H4-2-CH2NMe2)P}M·1/2OEt 2 [Ar = mes, M = Na (8), K (9); Ar = Tripp, M = K (10)]. Metathesis reactions between 9 and LaI3(THF)4 give only intractable products; in contrast, a metathesis reaction between 10 and LaI 3(THF)4 yields the heteroleptic complex {(Tripp)(C 6H4-2-CH2NMe2)P}2LaI (11). Compound 11 reacts cleanly with K{N(SiMe3)2} to give {(Tripp)(C6H4-2-CH2NMe2)P} 2La{N(SiMe3)2} (14). Compounds 3-5, 8-11 and 14 have been characterised by multi-element NMR spectroscopy; in addition, compounds 5, 11 and 14 have been studied by X-ray crystallography. The Royal Society of Chemistry 2006.
