Continuous Flow Synthesis of Methanofullerenes in Microstructured Reactors: A Kinetic Study

The kinetics of the cyclopropanation reaction of diethyl malonate with [60]fullerene were assayed to optimize the continuous flow synthesis of the methanofullerene monoadduct. Experiments were carried out under both batch and flow conditions, by sampling the reaction mixture at different times and separating the components by means of HPLC in a way that resembles a stop/quenched flow system with the addition of a chromatographic step before analysis. The observed concentration profiles of the fullerene species in the reaction mixture were used to calculate the pertinent rate constants and to optimize the selectivity towards the monoaddition product. A simple fluidic setup for the continuous production of methanofullerenes allowed kinetic studies to be performed on this fast process and its selectivity to be optimized.