About: Synthesis and characterisation of trimethylsilyl phosphorohalidates Me3SiOP(O)FX (X=Cl,Br) and (Me3SiO)2P2O3F2     Goto   Sponge   NotDistinct   Permalink

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  • Trimethylsilyl phosphorochloridofluoridate, Me3 SiOP(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 Me3 SiOP(O)FBr is formed in an analogous reaction of POFBr2 with (Me3 Si)2 O, however its susceptibility to spontaneous decomposition makes its isolation unfeasible. Condensation of Me3 SiO-P( O)FCl with (Me3 SiO)2 P(O)F or heating of POFBr2 with excess hexamethyldisiloxane gave bis(trimethylsilyl) diphosphorodifluor-idate, (Me3 SiO)2 P2 O3 F2 , in 45 to 53% yield. The existence of both expected diastereoisomers was revealed by 19 F and 31 P NMR spectroscopy.
  • Trimethylsilyl phosphorochloridofluoridate, Me3 SiOP(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 Me3 SiOP(O)FBr is formed in an analogous reaction of POFBr2 with (Me3 Si)2 O, however its susceptibility to spontaneous decomposition makes its isolation unfeasible. Condensation of Me3 SiO-P( O)FCl with (Me3 SiO)2 P(O)F or heating of POFBr2 with excess hexamethyldisiloxane gave bis(trimethylsilyl) diphosphorodifluor-idate, (Me3 SiO)2 P2 O3 F2 , in 45 to 53% yield. The existence of both expected diastereoisomers was revealed by 19 F and 31 P NMR spectroscopy. (en)
  • 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. (cs)
Title
  • Synthesis and characterisation of trimethylsilyl phosphorohalidates Me3SiOP(O)FX (X=Cl,Br) and (Me3SiO)2P2O3F2
  • Synthesis and characterisation of trimethylsilyl phosphorohalidates Me3SiOP(O)FX (X=Cl,Br) and (Me3SiO)2P2O3F2 (en)
  • Syntéza a charakterizace trimethylsilylhalogenofosforečnanů Me3SiOP(O)FX (X=Cl,Br) a (Me3SiO)2P2O3F2 (cs)
skos:prefLabel
  • Synthesis and characterisation of trimethylsilyl phosphorohalidates Me3SiOP(O)FX (X=Cl,Br) and (Me3SiO)2P2O3F2
  • Synthesis and characterisation of trimethylsilyl phosphorohalidates Me3SiOP(O)FX (X=Cl,Br) and (Me3SiO)2P2O3F2 (en)
  • Syntéza a charakterizace trimethylsilylhalogenofosforečnanů Me3SiOP(O)FX (X=Cl,Br) a (Me3SiO)2P2O3F2 (cs)
skos:notation
  • RIV/00216224:14310/04:00010078!RIV08-MSM-14310___
http://linked.open.../vavai/riv/strany
  • 83-90
http://linked.open...avai/riv/aktivita
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  • Z(MSM 143100011)
http://linked.open...iv/cisloPeriodika
  • 1
http://linked.open...vai/riv/dodaniDat
http://linked.open...aciTvurceVysledku
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  • 589316
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  • RIV/00216224:14310/04:00010078
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  • Trimethylsilyl esters; Phosphorochloridofluoridate; Phosphorobromidofluoridate; Diphosphorodifluoridate; Condensation reations; Thermal decomposition (en)
http://linked.open.../riv/klicoveSlovo
http://linked.open...odStatuVydavatele
  • GB - Spojené království Velké Británie a Severního Irska
http://linked.open...ontrolniKodProRIV
  • [65EEE02B37D8]
http://linked.open...i/riv/nazevZdroje
  • Journal of Fluorine Chemistry
http://linked.open...in/vavai/riv/obor
http://linked.open...ichTvurcuVysledku
http://linked.open...cetTvurcuVysledku
http://linked.open...UplatneniVysledku
http://linked.open...v/svazekPeriodika
  • 125
http://linked.open...iv/tvurceVysledku
  • Rovnaník, Pavel
  • Černík, Miloš
http://linked.open...n/vavai/riv/zamer
issn
  • 0022-1139
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  • 14310
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