Matrix-assisted laser desorption - time-of-flight mass spectroscopy

In this context, dialdehyde la (5 mg, 0.017 mmol), sarcosine (14 mg, 0.157 mmol) and five-fold excess of Ceo (60 mg, 0.083 mmol) dissolved in 10 ml of o-dichlorobenzene (o-DCB) heated at 130 °C for 90 min. After a typical work up procedure, the reaction mixture is purified by recycling HPLC on a preparative Buckyprep Cosmosil column (250 X 20 mm, toluene eluent, lOml/min flow rate) to furnish bis-fullerene derivative 3 in 32 % yield. The bis-fullerene 3 shows moderate solubility, thus allowed us to record and NMR spectra (Supp. Info., Fig. SI) corroborating the depicted structure in Scheme 1. The attenuated-total-reflectance infra-red (ATR-IR) spectrum of 3 demonstrates the characteristic stretching vibrations of the C-H (2803-3030cm" ) as well as the characteristic absorptions for fullerenes (Supp. Info., Fig. S2). Matrix-assisted-laser-desorption time-of-flight mass-spectroscopy (MALDI-TOF-MS), in the negative ionization mode and with the aid of trans-2-[3-(4-tert-butylphenyl)-2-methyl-2-propenylidene]malononitrile shows the molecu-... 

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