PREPARATION OF HYDROFULLERENES BY HYDROGEN RADICAL-INDUCED HYDROGENATION

Fullerite (a mix of crude C60 and C70) has been hydrogenated using hydrogen radical species (H.) at elevated temperatures (400-degrees-C) and hydrogen pressures (6.9 MPa (cold)). Iodoethane was employed as the hydrogen radical promoter. Analysis of the reduced fullerite by fast atom bombardment mass spectrometry revealed a mixture of hydrofullerenes comprising mainly C60H36 and C70H36. No spectral evidence for the ethylation or iodination of the fullerite was found. Prepared under these conditions, the product is only sparingly soluble in common solvents. Solid-state C-13 nuclear magnetic resonance spectroscopy and infrared spectroscopy were used to characterize the reduced fullerite. The structure of the C60H36 produced under these conditions is of lower symmetry than T(h) and most likely D3d or C3i symmetry.