New ferrocenylmethylphosphines – Preparation, characterisation and coordination chemistry of PH(CH2Fc)2, P(CH2Fc)3 [Fc=Fe(η5-C5H5)(η5-C5H4)] and their derivatives
摘要:
The new ferrocenylmethylphosphines PH(CH(2)Fc)(2) (1) [Fc=Fe(eta(5)-C5H5)(eta(5)-C5H4)] and P(CH(2)Fc)(3) (2) and the phosphonium salt [P(CH(2)Fc)(3)(CH2OH)]I (3) were synthesised from P(CH2OH)(3) and [FcCH(2)NMe(3)]I. [P(CH(2)Fc)(CH2OH)(3)]Cl (4) was obtained from P(CH(2)Fc)(CH2OH)(2), CH2O and HCl. The new phosphines and phosphonium salts were fully characterised by NMR and IR spectroscopy and MS. [Mo(CO)(6)] reacts with 1 to give [Mo(CO)(5){PH(CH(2)Fc)(2)}] (5) in high yield, but attempts to employ 2 as a ligand failed. The reaction of [P(CH(2)Fc)(3)(CH2OH)]I (3) and [PH(CH(2)Fc)(3)]I (obtained in situ from 3 and Na2S2O5) with [WI2(CO)(3)(NCMe)(2)] gave the complex salts [P(CH(2)Fc)(3)(CH2OH)][WI3(CO)(4)] (6) and [PH(CH(2)Fc)(3)][WI3(CO)(4)] (7), respectively. [P(CH(2)Fc)(4)]I (8) was synthesized from PH(2)CH(2)Fc and [FcCH(2)NMe(3)]I. Crystal structures were obtained for 1, 3 - 8. (C) 2007 Elsevier B. V. All rights reserved.