Abstract Preparation and properties of a [1,3,4]thiazaphospholidine are described. The 31P. 13C and 1H NMR spectra in double and triple resonance mode are recorded and discussed in detail.
Bis[bis(diethylamino)difluorphosphoranyl]acetylen, 4, bildet mit der äquimolaren Menge BF3 · Ether das nur bei niedrigen Temperaturen stabile Phosphonium‐tetrafluoroborat 7, das durch seine NMR‐Spektren und die Ergebnisse einer Röntgenstrukturanalyse charakterisiert wird. Mit der doppelt molaren Menge BF3 · Ether bildet 4 das Diphosphonium‐bis(tetrafluoroborat) 8. Bis[bis(diethylamino)phosphanyl]acetylen wird von Tetrachlor‐o‐benzochinon zu Verbindung 6 oxidiert.
Abstract Bis(diethylamino)phosphanylacetylen reacts with N.N′-dimethyl thiourea to give 2-diethyl-amino-1,4-dimethyl-3-methylene-[1,4,2]diazaphospholidine-5-thion (2) besides the [1,3,4]thiazaphospholidine (1). The latter compound is converted into 2 by heating. Reaction of 2 with various reagents yields other members of the title compound class. All new compounds are characterized by some reactions and their NMR and IR spectra. In addition, the results of an X-ray structure analysis of 2-diethylamino-l ,4-dimethyl-3-methylene-2-thioxo-[1,4,2]diazaphos-pholidine-5-thion (5) are reported.
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