Abstract In this note, we reported a new synthetic method for the preparation of water-soluble fullerol (60% yield) by the reaction of C 60 n− lithium salt with the acidified methanol/water solution in the presence of oxygen. The elemental analysis showed an average composition of C 60H 2(OH) 24. The FAB–MS spectrum displays a base peak for C 60 at 720 (m/z), whereas the product's molecular ion peak was not detected. In contrast to the pure C 60, this material exhibits interesting paramagnetic properties. An unusual temperature dependence for the ESR spectrum is observed over the temperature range 300–450 K. This change is irreversible.