Varian gemini 200 mhz

Fullerenol C₆₀(OH)₃₆ was synthesized from fullerene C₆₀ (99.5%). Sodium hydroxide, perhydrol (H₂O₂, 30%) and Amberlit MB20 were used for the synthesis of fullerene. Polyhydroxylated fullerene was obtained using the method described previously by Krokosz et al. [67 (link)]. First, fullerene C₆₀ was reacted with solid NaOH and perhydrol (H₂O₂, 30%) at room temperature. Hydrolysis was carried out for 24 h. Fullerenol was precipitated with methanol. Subsequently, NaOH residues were removed by ion-exchange chromatography on AmberlitMB-20. The structure of the obtained C₆₀OH₃₆ was confirmed by IR spectrophotometry (NEXUS FT-IR spectrometer, Thermo Fisher Scientific, Waltham, MA, USA), ¹H-NMR (Varian Gemini 200 MHz, Varian Inc., Palo Alto, CA, USA ), ¹³C-NMR (Bruker Avance III 600 MHz, Bruker Corp., Billerica, MA, USA), and mass spectroscopy MS-ESI (Varian 500 MS, Varian Inc., Palo Alto, CA, USA).

Fullerenol (polyhydroxyfullerene) C₆₀(OH)₃₆ was synthesized by the solvent-free method proposed by Wang et al. [53 (link)], and, in a modified version was described in the previous paper of Grebowski et al. [50 (link)]. Fullerenol was prepared by grinding pristine fullerene C₆₀ with NaOH and 30% hydrogen peroxide in a glass mortar in air at room temperature for 25 min (Wang et al. recommended 15 min), then the additional incubation of the reaction mixture at 60 °C (water bath) was carried out for 20 min. The crude mixture was dissolved in 50 mL of deionized water and hydrolysis was performed for 24 h. Fullerenol was precipitated with methanol, resolubilized with water, and traces of NaOH were removed by passing the solution over the ion exchange resin (Amberlit MB-20). The structure of the obtained hydroxyl derivative of fullerene C₆₀ was confirmed by IR spectrophotometry (EXUS FT-IR spectrometer, Thermo Fisher Scientific, Waltham, MA, USA), ¹H-NMR (Bruker Avance III 600 MHz, Bruker Corp., Billerica, MA, USA), ¹³C-NMR (Varian Gemini 200 MHz, Varian Inc., Palo Alto, CA, USA), MALDI-TOF/TOF mass spectrometry (Axima Performance Mass Spectrometer, Shimadzu Biotech, Kyoto, Japan) as described previously [35 (link)].