ROVNANÍK, Pavel and Miloš ČERNÍK. Synthesis and characterisation of trimethylsilyl phosphorohalidates Me3SiOP(O)FX (X=Cl,Br) and (Me3SiO)2P2O3F2. Journal of Fluorine Chemistry. Velká Britanie: Elsevier B.V., 2004, vol. 125, No 1, p. 83-90. ISSN 0022-1139.
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Basic information
Original name Synthesis and characterisation of trimethylsilyl phosphorohalidates Me3SiOP(O)FX (X=Cl,Br) and (Me3SiO)2P2O3F2
Name in Czech Syntéza a charakterizace trimethylsilylhalogenofosforečnanů Me3SiOP(O)FX (X=Cl,Br) a (Me3SiO)2P2O3F2
Authors ROVNANÍK, Pavel (203 Czech Republic) and Miloš ČERNÍK (203 Czech Republic, guarantor).
Edition Journal of Fluorine Chemistry, Velká Britanie, Elsevier B.V. 2004, 0022-1139.
Other information
Original language English
Type of outcome Article in a journal
Field of Study 10402 Inorganic and nuclear chemistry
Country of publisher United Kingdom of Great Britain and Northern Ireland
Confidentiality degree is not subject to a state or trade secret
Impact factor Impact factor: 1.364
RIV identification code RIV/00216224:14310/04:00010078
Organization unit Faculty of Science
UT WoS 000188380000013
Keywords in English Trimethylsilyl esters; Phosphorochloridofluoridate; Phosphorobromidofluoridate; Diphosphorodifluoridate; Condensation reations; Thermal decomposition
Tags Condensation reations, Diphosphorodifluoridate, Phosphorobromidofluoridate, Phosphorochloridofluoridate, thermal decomposition, Trimethylsilyl esters
Changed by Changed by: RNDr. Miloš Černík, CSc., učo 2255. Changed: 26/1/2005 15:49.
Abstract
Trimethylsilyl phosphorochloridofluoridate, Me3SiOP(O)FCl, has been prepared by reaction of POFCl2 with hexamethyldisiloxane or by treatment of bis(trimethylsilyl) phosphorofluoridate with phosphorus pentachloride. The compound could be purified by vacuum distillation and has been isolated in 55% yield. The ester Me3SiOP(O)FBr is formed in an analogous reaction of POFBr2 with (Me3Si)2O, however, its susceptibility to spontaneous decomposition makes its isolation unfeasible. Condensation of Me3SiOP(O)FCl with (Me3SiO)2P(O)F or heating of POFBr2 with excess hexamethyldisiloxane gave bis(trimethylsilyl) diphosphorodifluoridate,(Me3SiO)2P2O3F2,in 45 to 53% yield. The existence of both expected diastereoisomers was revealed by 19 F and 31 P NMR spectroscopy.
Abstract (in Czech)
Trimethylsilylester kyseliny chlorofluorofosforečné,Me3SiOP(O)FCl,byl připraven reakcí POFCl2 s hexamethyldisiloxanem nebo působením chloridu fosforečného na bis(trimethylsilyl)fluorofosfát. Sloučenina mohla být přečistěna vakuovou destilací a byla izolována v 55% výtěžku. Ester Me3SiOP(O)FBr se tvoří v obdobné reakci POFBr2 s (Me3Si)2O, avšak jeho sklon k samovolnému rozkladu znemožňuje jeho izolaci. Kondenzace Me3SiOP(O)FCl s (Me3SiO)2P(O)F, nebo zahřívání POFBr2 s nadbytkem hexamethyldisiloxanu, poskytly bis(trimethylsilyl)ester kyseliny difluorodifosforečné, (Me3SiO)2P2O3F2, ve výtěžku 45 až 53%. Existence jeho obou očekávaných diastereoizomerů byla potvrzena 19 F a 31 P NMR spektroskopií.
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MSM 143100011, plan (intention)Name: Struktura a vazebné poměry, vlastnosti a analýza syntetických a přírodních molekulových ansamblů
Investor: Ministry of Education, Youth and Sports of the CR, Structure and character of bonding, properties and analysis of synthetic and natural molecular ensembles
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