[PDF][PDF] The synthesis of hexafluorosumanene and its congeners

BM Schmidt, B Topolinski… - … -A European Journal, 2013 - researchgate.net
BM Schmidt, B Topolinski, S Higashibayashi, T Kojima, M Kawano, D Lentz, H Sakurai
Chemistry-A European Journal, 2013researchgate.net
All experiments were carried out under standard Schlenk conditions and argon atmosphere,
with commercially available anhydrous solvents. Melting points were determined on a
Stanford Research Systems MPA100 and are uncorrected. IR spectra were recorded on a
JASCO FT IR-4100 spectrometer (signals are denoted as following, s (strong), m (middle)
and w (weak)). UV spectra were recorded on a JASCO V-670 spectrometer, fluorescence
spectra were recorded on a JASCO FP6500 spectrometer. 1H, 19F and 13C NMR spectra …
All experiments were carried out under standard Schlenk conditions and argon atmosphere, with commercially available anhydrous solvents. Melting points were determined on a Stanford Research Systems MPA100 and are uncorrected. IR spectra were recorded on a JASCO FT IR-4100 spectrometer (signals are denoted as following, s (strong), m (middle) and w (weak)). UV spectra were recorded on a JASCO V-670 spectrometer, fluorescence spectra were recorded on a JASCO FP6500 spectrometer. 1H, 19F and 13C NMR spectra were measured on JEOL ECS 400/500 spectrometer or on a Bruker Instruments AVIII 700 at 23 C. CDCl3 and CD2Cl2 were used as solvents and the residual solvent peak was taken as an internal standard (1H NMR: CDCl3 7.26; 13C NMR: CDCl3 77.0 ppm; always proton-decoupled), 19F NMR spectra were referenced against external CFCl3. High resolution mass spectra (HRMS) were measured on a JEOL JMS-777V spectrometer using electron impact ionization method (EI). TLC analysis was performed using Merck Silica gel 60 F254 and PTLC was conducted using Wako Wakogel B-5F. All reagents and solvents were commercially purchased and used as received.
Pyridine Hydrofluoride (Olah’s Reagent, HF-py), density 1.1, available from Sigma-Aldrich, a 7: 3 w/w mixture of anhydrous HF and pyridine with a molecular weight of 263 gmol-1, formulated as C5H5N (HF) 9.2, as proposed by Umemoto and co-workers [S1] was used for stoichiometric calculations.
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