Developmental Research on Scale-up in Electrochemical Fluorination

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Developmental Research on Scale-up in Electrochemical FluorinationThis research consists of mainly two programs. The first is development of new electrochemical perfluoromethylation of olefins in a small sacle reactions and the second is a scale-up electrolysis of electrochemical trifluoromethylation, of methyl acrylate in 0. I kg scale by a flow cell electrolysis system.Electrochemical perfluoroalkylations of methyl acrylate, acrylamide, and acrylonitrile have been investigated. Perfluorooctanoic, butanoic, and difluoroacetic acids provided dimers of the corresponding perfluorinated carbon radicals in reasonable yields. In the oxygen atmosphere the electrolysis gave 2-oxo or. 2-hydroxy-4, 4, 4-trifluorobutylates in 30 - 45 % yields. This oxy-trifluoromethylation is promising for preparation of some valuable trifluoromethyl compounds otherwise difficult to prepare.A flow cell equipped with 10 X 10 cm^2 platinated titanium plates as electrodes was employed for 0. I Kg scale electrolysis of TFA and methylacrylate to give 50 % of the desired products at the current densities of 50 - 80 mA/cm^2. The temperature of the electrolysis affects current efficiency intensively. The lower temperature at around 0 C is desirable for the purpose.