A selective anodic oxidation system in which a carbocation intermediate is generated exclusively by use of a temperature-controlled multiphase solution to separate the different stages of the reaction from each other and from the products is described. The formation of a thermomorphic middle layer in an electrolytic solution composed of c-Hex and LPC/MeNO2 results in enhanced interaction between aliphatic alkenes and polar unstable cation.

Solution. -Electrolysis of phenols in the presence of unactivated alkenes using a temperature-controlled three-phase solvent system gives the desired cycloaddition products. The solvent system separates the different stages of the reaction (selective carbocation generation, C-C bond formation) and the products from each other. The formation of a thermomorphic middle layer composed of cyclohexane/ LiClO 4 / MeNO2 results in enhanced interaction between aliphatic alkenes and polar unstable cation. -(KIM, S.; NODA, S.; HAYASHI, K.; CHIBA*, K.; Org.