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Seven‐Minute Synthesis of Pure C s ‐C 60 Cl 6 from [60]Fullerene and Iodine Monochloride: First IR, Raman, and Mass Spectra of 99 mol % C 60 Cl 6
Author(s) -
Kuvychko Igor V.,
Streletskii Alexey V.,
Popov Alexey A.,
Kotsiris Sotirios G.,
Drewello Thomas,
Strauss Steven H.,
Boltalina Olga V.
Publication year - 2005
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.200500185
Subject(s) - chemistry , toluene , raman spectroscopy , yield (engineering) , high performance liquid chromatography , iodine monochloride , benzene , mass spectrometry , mass spectrum , analytical chemistry (journal) , column chromatography , solvent , fullerene , chromatography , iodine , organic chemistry , materials science , physics , optics , metallurgy
Three previously reported procedures for the synthesis of pure C s ‐C 60 Cl 6 from C 60 and ICl dissolved in benzene or 1,2‐dichlorobenzene were shown to actually yield complex mixtures of products that contain, at best, 54–80 % C s ‐C 60 Cl 6 based on HPLC integrated intensities. MALDI mass spectrometry was used for the first time to identify other components of the reaction mixtures. An improved synthetic procedure was developed for the synthesis of about 150 mg batches of chlorofullerenes containing 90 % C s ‐C 60 Cl 6 based on HPLC intensities. The optimum reaction time was decreased from several days to seven minutes. Small amounts of the product were purified by HPLC (toluene eluent) to 99 % purity. The pure compound C s ‐C 60 Cl 6 is stable for at least three months as a solvent‐free powder at 25 °C. The Raman, far‐IR, and MALDI mass spectra of pure C s ‐C 60 Cl 6 are reported for the first time. The Raman and far‐IR spectra, the first reported for any C 60 Cl n chlorofullerene, were used to carry out a vibrational analysis of C s ‐C 60 Cl 6 at the DFT level of theory.