Trichonnethylphosphonsäuredihydrazid und 3.6-Bi8(trichlormethyl)-3.6-dioxo-1.2.4.5-tetraaza-3.6-diphosphacyclohexan / Trichloromethylphosphonic Acid Dihydrazide and 3,6-Bis(trichloromethyl)-3,6-dioxo-1,2,4,5-tetraaza-3,6-diphosphacyclohexane

Abstract

Abstract The title compounds are prepared from trichloromethylphosphonic acid dichloride and excess hydrazine hydrate, and from the dihydrazide and the dichloride in the presence of triethylamine, resp. They are characterized by elemental analysis, mass spectra, 1H and 31P NMR spectra, IR and Raman data. Thin layer chromatographic experiments show that in the raw material of the ring compound two isomers (probably cis- and trans-) are present, whereas in the recrystallized product only one isomer can be detected. Attempts of a preparative separation of isomers were unsuccessfull so far due to very low concentrations of the product with the slightly higher Rf. Single crystals of the isolated ring compound decompose on irradiation with X-rays