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Reaction of N,N′-dimethyl-N,N′-bis(trimethylsilyl)urea (1) with dichlorophosphines. RPCl 2  (R = Et: 14; R = Pr: 15) has furnished the P-chloro-substituted acyclic diphosphorus compounds, 16 and 17. In the analogous reaction of 1 with Ph 2 PCl the corresponding bis(diphenylphosphino)-substituted derivative, 21 was formed. Dehalogenation of 11, 16 and 17 with oxalic acid bis(trimethylsilyl) ester, 22 has produced the mixed-valent cyclic λ 3 P,λ 4 P-diphosphorus compounds, 23-25 in almost quantitative yield. Oxidation of the λ 3 P atom in 23-25 with tetrachloroorthobenzoquinone, 26 has given rise to partial cleavage of the P-P bond, and only moderate yields of the products, 29, 31 and 32, have been obtained. The characterization of the various compounds obtained rests, especially, on their  1 H and  31 P NMR spectra, and on a study of their mass spectral fragmentation pattern

zeitschrift für naturforschung b

Über die Darstellung von P-Chlor-substituierten Ν,N′-Dimethylharnstoff-verbrückten Diphosphorverbindungen, deren Enthalogenierung mit Oxalsäurebis(trimethylsilylester) und anschließende Oxidation mit Tetrachlororthobenzochinon / Preparation of P-Chloro-Substituted N′,N′-Dimethylurea-Bridged Diphosphorus Compounds, their Dehalogenation with Oxalic Acid Bis(trimethylsilyl) Ester and Subsequent Oxidation with Tetrachloroobenzoquinone