Synthesis and characterization of some 2H-1,4,2-diazaphosphole-, 2H-1,3,2-diazaphosphole- and 2H-1,2-diazaphosphole-P-sulfide derivatives

Partial decomplexation of 2H-1,4,2-diazaphosphole and 2H-1,2-azaphosphole c omplexes is observed upon prolonged heating in benzonitrile; the liberated heterocycles were detected spectroscopically, but could not be isolated. Th e first 2H-1,3,2-diazaphosphole derivative, formed by thermal decomplexatio n using o-xylene and 1,2-bis(diphenylphosphino)ethane, was isolated and cha racterized. In all three cases, the corresponding heterocyclic P(V)-sulfide s were obtained by oxidative decomplexation using elemental sulfur. All pro ducts were characterized by NMR and MS spectroscopy and two, additionally, by X-ray diffraction. (C) 1999 Elsevier Science Ltd. All rights reserved.