Ammonium thiophosphate

E. Glatzel was unable to make normal ammonium thiophosphate, (NH4)8PS4,... 

The triamide, SP(NH2)s, was prepared by saturating PSC13 with ammonia. It was a white solid of density 1-7. When heated it dissociated into ammonium sulphide and sulphur, leaving phosphorus in the residue, probably as phospham, and was decomposed by warm water giving H2S and ammonium thiophosphate. It was only slightly soluble in alcohol or carbon disulphide. 

This compound is formed together with sal-ammoniac ly the action of ammonia upon phosphoms thiochlmide. It exists as a white amorphous mass whi[Pg.518]

Thus the condensation of dichloroether or chloroacetone fails to give the parent compound, 2-hydroxythiazole (158a), Rj = R2 = R3 = H (221). However, 2-hydroxythiazole can be obtained in 12% yield from chloro-acetaldehyde (386). The condensation of ammonium thiocarbamate with cf-chloroketones gives the corresponding 2-hydroxy derivatives in 25 to 70% yields (76, 221, 304, 412) (Table 11-24). These compounds condensed with ClP(S)(OEt)2 give the corresponding 2-thiazolyl-thiophosphates (791). 

Trlammoninm imidotrithio- Diammonium lmidotri- Ammonium imidotrithio- Imidotrithiophosphoric phosphate. thiophosphate. phosphate. acid. 

P0SC12(C2II5) 0-Ethyl dichloro-thiophosphate, 4 75 P02F2NH4 Ammonium difluoro-phosphate, 2 157... 

Trisodium dithiophosphate, Na3(PS202).llH20, has been prepared from P2S6 and a rather concentrated solution of sodium hydroxide. The solution was heated to 50° to 55° C. until the trithio-salt was decomposed. The salt was precipitated by alcohol, and when re-crystallised from water appeared as colourless six-sided prisms.5 The ammonium salt, (NH4)3(PS202).2H2O, was prepared similarly from aqueous ammonia and P2S5. From these soluble thiophosphates those of the heavy metals may be obtained by double decomposition.5... 

Thiophosphates, Detection.—Many of the reactions already described, such as the production of H2S and phosphoric acid when these salts are treated with acids, will serve to detect the thiophosphates. The alkali and ammonium salts are soluble, the others mostly insoluble. Calcium, barium and strontium monotbiophosphates, barium and strontium dithiophosphates and barium trithiophosphate are insoluble, the other alkaline earth salts soluble. Thiophosphate solutions mixed with alkali sulphides give a green colour with ferric chloride. Monothiophosphates give a blue precipitate with cobalt sulphate soluble in excess of the cobalt salt, dithiophosphates a green precipitate soluble in excess of dithiophosphate, and trithiophosphates a brown solution. Several other tests have been described.3... 

Di- and Tri-imido- and -amido-thiophosphates.—A great variety of these compounds, chiefly in the form of their ammonium salts, was obtained by the action of ammonia, usually in the liquid form, on phosphorus pentasulphide.5 Some of the ammonia could be driven off by heating under reduced pressure, leaving the acid salts. 

Reactions of alkyl halides with diethyl phosphite in the presence of ammonium acetate/sulfur and acidic aluminia using microwave irradiation provide a simple and general route to thiophosphates. Two diastereoisomers of 1,3,2-dithiadiphosphetane 2-sulfide (19) have been isolated for the first time via the reaction of thioketones (20) with Lawesson s reagent (Figure 5). ... 

POSCl2(C2H5) 0-Ethyl dichloro-thiophosphate, 4 75 POS(NH)2Na Sodium diimido-thiophosphate, 6 112 PO2F2NH4 Ammonium difluoro-phosphate, 2 157 P03(C2H5)2H Diethyl phosphite, 4 58... 

Isothiouronium and quaternary ammonium 0,S-dimethyl thiophosphates from thionophosphoric acid esters s. 16, 645... 

A soln. of trimethyl thionophosphate and thiourea in abs. alcohol heated 5 hrs. in a water bath S-methylisothiouronium 0,S-dimethyl thiophosphate. Y 96.5%.— Also quaternary ammonium 0,S>dimethyl thiophosphates from tert. amines s. G. Hilgetag and H. Teichmann, J. pr. 8, 90 (1959). 

Quaternary ammonium salts Metho-0,S-dimethyl thiophosphates... 

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