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Phản ứng của NF4+SbF6− với các muối nitrate kim loại kiềm trong dung môi CH3CN hoặc SO2 ở nhiệt độ thấp, sẽ tạo thành FONO2.
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In the dry box, equimolar amounts (1.00 mmol each) of NF4SbF6 and CsNO3 were placed into a prepassivated (with ClF3) Teflon ampoule. This ampoule was then connected to the Pyrex glass line, and dry CH3CN (3 ml liquid) was condensed in at −196°C. It was then connected to the steel vacuum line, and the reaction mixture was warmed to −40°C. Upon melting of the solvent, strong gas evolution was observed. The turbid solution was stirred for 15 min, and the volatile products were separated by fractional condensation in a dynamic vacuum through three cold traps, kept at −126 (methylcyclohexane slush bath), −183 (liquid oxygen), and −210°C (nitrogen slush), respectively. The −126°C trap contained the CH3CN solvent, the −183°C trap had 1.0 mmol of pure FONO2 that was identified by its vibrational [6 and 7] and 19F NMR [8] spectra, while the −210°C trap contained 1.0 mmol of NF3. The nonvolatile white solid residue in the ampoule consisted of 1.0 mmol of CsSbF6 that was identified by its Raman spectrum [9].
When in the above reaction the CH3CN solvent was replaced by SO2 and the reaction was carried out at the melting point of SO2 (approx. −70°C), again quantitative FONO2 and NF3 evolution was observed. However, the separation of the FONO2 from the SO2 solvent was more difficult due to their more similar volatilities.