E. K. Badeeva

New Method for the Preparation of Octathiotetraphosphetanes on the Basis of Elemental Phosphorus and Sulfur: Structure and Properties

Abstract New octathiotetraphosphetane ammonium salts are obtained based on the reaction of white phosphorus (Р4) and elemental sulfur with aliphatic mercaptans in the presence of amines (morpholine, methylmorpholine, pyrrolidine, and N,N-dimethylbenzylamine). The salts of octathiotetraphosphetane are characterized by IR/Raman spectroscopy. Several common IR and Raman bands can be used as structural markers for establishing the structures of [P4S8]4− anion in new compounds.

Coordination Features of P,S-Ligands Based on the Phosphorus Derivatives with I and Viii Group Metals

Abstract Continuing the study of the coordination ability of P,S-ligands, we have investigated the behavior of some P(IV)-S-phosphorus derivatives, in particular, trialkyltetrathiophosphates (R = i-Pr, Bu) and piperidinium and triethylammonium salts of octathiotetraphosphetane in reaction with Cu(I), Ag(I), Co(II), and Fe(II) halides. The series of complexes were obtained and characterized by the X-ray single crystal diffraction and IR/Raman spectroscopy. GRAPHICAL ABSTRACT

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

We have recently demonstrated that reactions of white phosphorus (P4) and elemental sulfur with proton-donating reagents easily proceed in the presence of amines [4–6], yielding ammonium salts of phosphorous and hypophosphorous acids and diesters of dithiophosphoric acid. 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. Extending the above-listed results, herein we demonstrate a new method to yield octathiotetraphosphetane via the reaction of P4, sulfur, and amines in the presence of 1,3-propanediol as protonodonor. The reaction was carried out in acetonitrile at 55–70oC during 8–10 h. The conversion of phosphorus was complete, and no hydrogen sulfide formation was observed. By cooling the reacted mixture down, we isolated compounds revealing the δP 120–122 ppm signal in P NMR spectra, identified as octathiophosphetane ammonium salts (Scheme 1).

Novel Effectively Carbonaceous and Sulfurated Hydrogen Corrosion Inhibitors on the Basis of Organosulfurphosphorus Compounds

Abstract Novel ammonium salts of O,O-dialkyl dithiophosphoric acids were obtained by one-pot synthesis from white phosphorus, elemental sulfur, industrial alcohols or phenols, and amines. Long-chain S-alkyl O,O-dialkyldithiophosphonates were prepared by the reaction of red phosphorus with elemental sulfur, alcohols, and the cheap industrial fractions of С16–С18 and С20–С26 of higher α-olefins in the presence of Lewis acid catalyst. The dithiophosphates obtained possess the high anticorrosion activities toward mild steel. GRAPHICAL ABSTRACT

Thermal stability of primary and secondary phosphine oxides formed as a reaction of phosphine oxide with ketones

GRAPHICAL ABSTRACT ABSTRACT We present the study of reactivity of electrochemically generated in situ from white phosphorus P4 phosphine oxide H3PO toward various ketones (acetone, methylethylketone, methyl-n-propylketone). This interaction was found to give a selective formation of mono- and bis-(α-oxyalkyl)phosphine oxides RR′C(OH)P(O)H2 (1) and (RR′C(OH))2P(O)H (2) where R = Me; R′ = Me, Et, n-Pr. Thermal properties of the formed primary and secondary phosphine oxides have been studied and quantum chemical calculations of thermodynamic stability of these compounds were performed.

Novel Approach to the Synthesis of Phosphorus Sulfur Organic Compounds and Their Metal Complexes

Abstract The reaction of elemental phosphorus (Pti 4) and sulfur with protonodonor reagents (alcohols, phenols, and thiols) has been studied in the presence of amines and complexes based on trialkyltrithiophosphites and transition metal halides. A novel approach to the synthesis of phosphorus sulfur organic compounds has been proposed on the basis of these reactions.

Octathiotetraphosphetanes – Novel Class of Biologically Active Phosphorusorganic Compounds. Synthesis, Structure, Properties

GRAPHICAL ABSTRACT ABSTRACT Reaction of white phosphorus with elemental sulfur and proton-donating reagents such as thiols and diols in the presence of different amines were studied. Octathiotetraphosphetane ammonium salts, ammonium salts of S,S′-dialkyltetratiophosphoric and O,O′-propylendithiophosphoric acids were obtained from the reactions. Red phosphorus reacted with sulfur and amines in the presence of microwave irradiation to form ammonium octathiotetraphosphetanes in high yields.