Publication result detail

Synthesis and charakterisation of trimethylsilyl phosphorohalidates: Me3SiO(O)FX (X= Cl, Br) and (Me3SiO)2P2O3F2.

ROVNANÍK, P.; ČERNÍK, M.

Original Title

Synthesis and charakterisation of trimethylsilyl phosphorohalidates: Me3SiO(O)FX (X= Cl, Br) and (Me3SiO)2P2O3F2.

English Title

Synthesis and charakterisation of trimethylsilyl phosphorohalidates: Me3SiO(O)FX (X= Cl, Br) and (Me3SiO)2P2O3F2.

Type

Peer-reviewed article not indexed in WoS or Scopus

Original 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 45-53 % yield. The existence of both expected diastereoisomers was revealed by 19F and 31P NMR spectroscopy.

English 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 45-53 % yield. The existence of both expected diastereoisomers was revealed by 19F and 31P NMR spectroscopy.

Authors

ROVNANÍK, P.; ČERNÍK, M.

Released

01.01.2004

ISBN

0022-1139

Periodical

JOURNAL OF FLUORINE CHEMISTRY

Volume

2004 (125)

Number

1

State

Swiss Confederation

Pages from

83

Pages to

90

Pages count

8

BibTex

@article{BUT44446,
  author="Pavel {Rovnaník} and Miloš {Černík}",
  title="Synthesis and charakterisation of trimethylsilyl phosphorohalidates: Me3SiO(O)FX (X= Cl, Br) and (Me3SiO)2P2O3F2.",
  journal="JOURNAL OF FLUORINE CHEMISTRY",
  year="2004",
  volume="2004 (125)",
  number="1",
  pages="83--90",
  issn="0022-1139"
}