A continuous electrochemical synthetic system has been developed using a cyclohexane-based multiphase electrolyte solution composed of lithium perchlorate and nitromethane. The upper cyclohexane phase functioned as both substrate supply and product assembly phases, whereas the electrochemical reactions took place in the lower electrolyte solution phase, achieving spatial separation of the electrolyte solution phase. (C) 2010 Elsevier Ltd. All rights reserved.