The results of the pretreatment behaviour and catalytic properties of sulfate-containing vanadyl pyrophosphate catalysts in the oxidation of n-butane to maleic anhydride (MA) are presented. It has been found that the increase in the MA selectivity during the pretreatment procedure of the fresh catalysts prepared by anaerobic calcination is mainly caused by the decrease in the catalytic activity for MA total oxidation. The change of the catalyst surface composition by oxidation of the surface layer and the site isolation resulting from surface termination in pyrophosphate groups as well as the change of the acidic properties during the pretreatment process using conventional butane/air mixtures are assumed to be the reasons for the above finding.

EPR studies of unsupported V2O5-Fe2O3 catalysts revealed that by doping with caesium sulfate a new phase is formed in the solids which apparently increases their selectivity in the catalytic oxidation of polycyclic hydrocarbons. The percentage of this phase rises with increasing iron content. As indicated by XRD and Mossbauer spectroscopy, the new phase is amorphous. Its composition is non-stoichiometric and Varies slightly depending on the iron content. For catalysts with V : Fe : Cs atomic ratios of 1 : 1 : 0.06 and 1 : 1.4 : 0.06, approximate formal compositions of Fe0.70VO3.04 and Fe0.65VO3.14, respectively, were calculated. A number of in situ EPR measurements performed with variation of temperature and atmosphere under mechanical stress and during treatment of the catalysts with fluorene, revealed that the active centres probably consist of oxygen lattice vacancies in the coordination spheres of Fe3+ ions which are occupied by an electron.

Some new results, especially on the fluoride degradation of phosphorus sulfides and phosphorus oxide sulfide are reported. Possible reaction mechanisms are discussed.

The title compounds may be regarded as a missing link in the series of planar 24-electron compounds Cl3B, Cl2CS, ClPS2, ClPO2, C1NO2, SO3. They are readily accessible by dissociation of betaine 1. The electron distribution in the compounds of this series is discussed on the basis of PE spectra. The positively charged centers are surrounded in a starlike fashion by substituents that are mostly negatively charged (X  O, S).

AbstractDie Reaktion von Py · PS2Cl (1; Py = Pyridin) mit primären aliphatischen Aminen im Molverhältnis 1:1 führt zu den Pyridiniumsalzen von 1‐Alkyl‐2‐alkylamino‐2, 4‐dithioxo‐1,3‐azathia‐2λ5, 4λ5‐diphosphetidinen (3), die mit MeI zu den entsprechenden Methylestern (4) reagieren. Im Fall des Cyclohexylaminderivates 4a ließen sich durch fraktionierte Kristallisation aus Cyclohexan das trans‐ und cis‐Isomere erhalten. Die Kristallstrukturen beider Isomeren wurden bestimmt. Kristalldaten: 4a(trans), triklin Raumgruppe P1, Z = 2, a = 11,028(5), b = 11,99(1), c = 7,706(7) Å, α = 86,06(7)°,: β = 101,54(5)°, γ = 82,86(5)°; 4a′(cis), triklin, Raumgruppe P1 Z = 2, a = 6,849(4), b = 13,37(1) Å, c = 15,446(8) Å, α = 110,01(7)°, β = 101,42(4)°, γ = 91,60(6)°.

Under definite conditions the dithiophosphoric acid chloride pyrididium betaine reacts with primary amines, RNH2, yielding four-membered rings. Depending on the electronic properties of R either diaza or thiazadiphosphetines are formed. An elimination-addition mechanism via imido dithiomonometaphosphate is discussed.

AbstractDie Reaktion des Dithiophosphorsäurechlorid‐pyrididiumbetains1mit bifunktionellen Nucleophilen eröffnet einen neuen Syntheseweg für 5‐ bzw. 6gliedrige cyclische Dithiophosphate (2a–i, 3, 5a–f). Synthese, spektroskopische Eigenschaften und Reaktionsverhalten dieser Stoffklasse werden beschrieben. Die Reaktion der cyclischen Dithiophosphate mit Alkylhalogeniden führt zu den entsprechenden S‐Alkylestern6a–o, deren massenspektroskopische Fragmentierung diskutiert wird.

Salts of the monofluorophosphoric acid, H2PO3F, has been studied first by LANGE [1]. By the reaction of Ag2PO3F and CuCl2·2H2O in aqueous solution GOSWAMI [2] has prepared a copper salt of the formula CuPO3F·5H2O.

AbstractDie Reaktion von P4O10 mit P4S10 führt zu einem Gemisch von Phosphoroxidsulfiden der allgemeinen Zusammensetzung P4O10−nSn. Die Anteile der einzelnen Phosphoroxidsulfide in diesem Reorganisationsgemisch lassen sich durch Änderung des Ausgangsmolverhältnisses P4O10/P4S10 variieren. Durch fraktionierte Destillation bzw. Kristallisation wurden neben dem bereits bekannten Oxidsulfid P4O6S4 erstmals die Verbindungen P4O7S3, P4O5S5, P4O4S6, P4O3S7 P4O2S8 und P4OS9 präparativ dargestellt sowie P4O8S2 NMR‐spektroskopisch identifiziert.

Chemischer InformationsdienstVolume 14, Issue 33 Reviews ChemInform Abstract: SYNTHESIS AND CONSTITUTION OF PHOSPHORUS CHALCOGENIDES WITH ADAMANTANE-LIKE STRUCTURE M. MEISEL, M. MEISELSearch for more papers by this author M. MEISEL, M. MEISELSearch for more papers by this author First published: August 16, 1983 https://doi.org/10.1002/chin.198333351Read the full textAboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article. Volume14, Issue33August 16, 1983 RelatedInformation

Dithiophosphoric acid chloride pyrididium betaine, Py. PS2Cl (1)1, can be widely used for the synthesis of various organophosphorus compounds. 1 reacts in the presence of a base with an excess of nucleophiles like amines, alcohols or thiols to the corresponding disubstituted thiophosphoric acid derivatives2–3.

Chemischer InformationsdienstVolume 14, Issue 38 Organoelement Compounds ChemInform Abstract: SYNTHESIS OF THE TRIMETHYLSILYL AMIDE OF DICHLOROTHIOPHOSPHORIC ACID ME3SIHNP(S)CL2 K. DOSTAL, K. DOSTALSearch for more papers by this authorJ. VESELA, J. VESELASearch for more papers by this authorM. MEISEL, M. MEISELSearch for more papers by this authorC. DONATH, C. DONATHSearch for more papers by this author K. DOSTAL, K. DOSTALSearch for more papers by this authorJ. VESELA, J. VESELASearch for more papers by this authorM. MEISEL, M. MEISELSearch for more papers by this authorC. DONATH, C. DONATHSearch for more papers by this author First published: September 20, 1983 https://doi.org/10.1002/chin.198338278Read the full textAboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article. Volume14, Issue38September 20, 1983 RelatedInformation

AbstractDie Reaktion von P4S10 oder P4S9 mit flüssigem Ammoniak führt unterhalb −33°C zu Ammoniumnonathiocyclotriphosphat, (NH4)3[P3S9] (I), das beim Abkühlen auf −78°C auskristallisiert. Bei der ammonolytischen Spaltung von I entsteht Amidotrithiophosphat, (NH4)2[PS3(NH2)]. Mit PCl3 reagiert I unter Rückbildung der Adamantanstruktur des P4S9. Weitere Eigenschaften und Reaktionen von I werden beschrieben.