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The electrochemical fluorination of 2-methyloxane, oxepane, 2-chloromethyloxane and 2-chloromethyloxolane has been carried out. The corresponding perfluoro(2-methyloxane) and perrfluorooxepane were obtained in fair yields from the first two compounds, but from the later two, the corresponding chlorine-containing perfluorocyclic ethers, i.e. perfluoro(2-chloromethyloxane) and perfluoro(2-chloromethyloxolane), were obtained only in small yields, respectively. These new compounds have been characterized by elemental analysis, and infrared, mass and 19F nmr spectra. 相似文献
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Minkwitz R Reinemann S Seelbinder R Konikowski D Hartl H Brüdgam I Hegge J Hoge B Sheehy JA Christe KO 《Inorganic chemistry》2001,40(17):4404-4408
In the superacidic HF/SbF(5) system, methyl trifluoromethyl ether forms at -78 degrees C the new tertiary oxonium salt [(CH(3))(2)OCF(3)](+)[Sb(2)F(11)](-), which was characterized by Raman and multinuclear NMR spectroscopy and its crystal structure. The same oxonium salt was also obtained by methylation of CH(3)OCF(3) with CH(3)F and SbF(5) in HF solution at -30 to -10 degrees C. Replacement of one methyl group in the trimethyloxonium cation by the bulkier and more electronegative trifluoromethyl group increases the remaining O-CH(3) bond lengths by 0.037(1) A and the sum of the C-O-C bond angles by about 4.5 degrees. Methylation of CH(3)OCF(CF(3))(2) with CH(3)F in HF/SbF(5) solution at -30 degrees C produces [(CH(3))(2)OCF(CF(3))(2)](+)[Sb(2)F(11)](-). The observed structure and vibrational and NMR spectra were confirmed by theoretical studies at the B3LYP/6-311++G(2d,2p) and the MP2/6-311++G(2d,p) levels. 相似文献
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The new salts NF4Be2F5 and NF4AlF4 were prepared from concentrated NF4HF2 solutions and BeF2 and AlF3 respectively. 相似文献
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Schroer T Haiges R Schneider S Christe KO 《Chemical communications (Cambridge, England)》2005,(12):1607-1609
The previous claim for the first generation of the pentazolate anion in solution was carefully reexamined; no evidence for the formation of cyclo-(N5-) was found under the reported conditions. 相似文献