- BEITRAEGE ZUR CHEMIE DER SCHEFELHALOGENIDE 15. DICHLOR-FLUOR-TRIFLUOROMETHYLSULFURAN, CF3SCl2F
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The preparation of the sulfurane CF3SCl2F is reported.Upon sublimation of the sulfonium salt CF3SCl2+AsF6- the compounds CF3SCl2F and AsF5 coexist in the gaseous phase.After trapping AsF5 as KAsF6 extremely instable CF3SCl2F is isolated and characterised by IR-, Raman- and 19F-NMR-spectroscopy.
- Minkwitz, Rolf,Nass, Ulrike
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p. 393 - 398
(2007/10/02)
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- Preparation and Chemical Properties of S-(Trifluoromethyl)-S,N-dihalosulfimides, (Trifluoromethylthio)(thiosulfinyl)amine, and Bis(trifluoromethyldithio)sulfur Diimide
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Oxidative halogenation of CF3SN(SiMe3)2 with F2 or Cl2 leads to CF3S(X)=NX (X=F, Cl) (2a, b).During the chlorination process CF3S(Cl)=NSiMe3 (3a) was isolated and characterized as an intermediate.It reacts with CF3SCl to give CF3S(Cl)=NSCF3 (3b) which was also obtained from (CF3S)2NH and Cl2 at -60 deg C.Similarly, CF3S(F)=NSCF3 (3c) was synthesized from (CF3S)2NH and F2 or from CF3SF3 and CF3SNH2. 3a-c decompose already at temperatures 5a, b).Analoguosly, CF3SN=S=NSCF3 (4b) reacts with cyclopentadiene to give 5c.Ringopening takes place during the reaction of + Cl- (6) with Hg(SCF3)2 with formation of CF3SSN=S=NSSCF3 (7) which was also obtained from (CF3SS)2NH and (ClSN)3 in the presence of pyridine.Physical and spectroscopic data of the compounds are reported.
- Haas, Alois,Walz, Ruediger
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p. 3248 - 3257
(2007/10/02)
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