Abstract
{[Tris(hydroxymethyl) methylamino]carbonyl} ferrocene (1) reacts with phosphorus(III) chloride in the presence of pyridine or triethylamine to afford a ferrocenyl-substituted bicyclic phosphite, {[(2,6,7-trioxa-1-phosphabicyclo[2.2.2] oct-4-yl) amino] carbonyl} ferrocene (2), in a moderate yield. (4,5-Dihydro- 4,4-bis(chloromethyl)-2-oxazolyl) ferrocene (3) is found to be formed in some experiments as a minor side-product, resulting presumably via halogenation of 1 and base-induced cyclization of an intermediate chloromethyl derivative. The reaction of 2 with [W(CO)(4)(cod)] (cod = cycloocta-1,5-diene) at elevated temperature produces bis-phosphite complex cis-[W(CO)(4)(2-kappa P)(2)] (4) as the major product.
All newly prepared compounds have been characterized by spectroscopic methods (IR, NMR and mass spectrometry) and elemental analysis. The crystal structures of 2, 3 center dot 1/2H(2)O and 4*Me2CO*H2O were determined by single-crystal X-ray diffraction and the redox behaviour of phosphite 2 and the W(0) complex 4 was studied by cyclic voltammetry.