Synthesis, IR/Raman, and quantum‐chemical structural analysis of new octathiotetraphosphetane ammonium salts

Abstract

New octathiotetraphosphetane ammonium salts are obtained based on the reaction of white phosphorus (P 4 ) and elemental sulfur with aliphatic mercaptans in the presence of amines (morpholine, methylmorpholine, pyrrolidine, and N,N-dimethylbenzylamine

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 The physico-chemical and the spectral parameters of the octathiotetraphosphetane ammonium salts 2a-c coincide with the same characteristics given in our previous publications. 5 Structures of salts 2a-c were confirmed by the XRD analysis as well.…”

“…5 The physico-chemical and the spectral parameters of the octathiotetraphosphetane ammonium salts 2a-c coincide with the same characteristics given in our previous publications. 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.…”

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.…”