Novel cyclic tetraphosphetanes: Molecular and crystal structures of diethylammonium and piperidinium salts of 1,2,3,4-tetramercapto-1,2,3,4-tetrathioxotetraphosphetane

Reaction of elemental phosphorus (P4) and sulfur with amines in the presence of alkylene glycols: New method to prepare octathiotetraphosphetane ammonium salts

“…The so formed crystals were filtered off, dissolved in acetonitrile, and precipitated with diethyl ether. Physico-chemical and spectral features of the products Ia-Ie agreed with the reference data [7,8]. IR spectra were recorded with the Bruker Tensor-27 Fourier spectrometer (KBr, 4000-400 cm -1 ).…”

“…Physicochemical and spectral parameters of the products Ia-Ie completely coincided with those of the compounds obtained via the reaction of P 4 , sulfur, and amines in the presence of thiols. The latter products were studied by IR, Raman, 31 P NMR, and 1 H NMR spectroscopy in combination with Density Functional Theory simulation; structure of the salts Ia-Ic was confirmed by X-ray diffraction analysis [7,8].R 1 = R 2 = Et (a); R 1 = H, R 2 = -(CH 2 ) 5 -(b); R 1 = H, R 2 = Et (c); R 1 = Me, R 2 = (CH 2 CH 2 ) 2 O (d); R 1 = CH 2 C 6 H 5 , R 2 = Me (e). P 4 R 1 NR 2 + P P P P S SH SH SH SH S S S…”

“…The reaction of white phosphorus and sulfur with aliphatic thiols in the presence of amines has been shown to give the fourmembered cyclic phosphorus compounds, ammonium salts of 1,2,3,4-tetramercapto-1,2,3,4-tetrathioxotetraphosphetane [7,8], with moderate yields. These salts were prepared previously [9,10] along with other cyclic thiophosphates via the reaction of white phosphorus with polysulfides, hydrogen sulfide, and amines.…”

New method for the synthesis of ammonium salts of O,O'-alkylenedithiophosphoric acid and octathiotetraphosphetane. Crystal structure features's of diethylammonium salt of O,O'-propylenedithiophosphoric acid

“…5 Structures of salts 2a-c were confirmed by the XRD analysis as well. 8, 9 It is relevant to note that these salts, as well as other cyclic thiophosphates, can also be obtained in reactions of white phosphorus with polysulfide polysulfides, hydrogen sulfide and amines. 6, 7 …”

“…Physical, analytical, and spectral data for 2c was given in previous publications. 9 The solution after filtration of salt 2c was then evaporated under reduced pressure to give red oil. Salt 1c was purified by column chromatography on silica gel.…”