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This study aimed to find reaction conditions that improve the yield of target intermediate products, using a two-phase system and a microspace for first-order consecutive and reversible reactions. As a result, the yield of target products with a two-phase system can be surpassed by that of a single-phase system through selecting the organic phase such that the partition coefficient of the raw material to the aqueous phase is large, and that of the target product to the organic phase is also large. In addition, the volume ratio of two phases and the liquid-liquid interfacial area are also important factors for improving the target product yield. In a microspace, the microfluid segments can be designed both arbitrarily and precisely, and thus it is possible to control the interfacial area and mass transfer rates accurately. Utilization of a microspace can play a significant role in intensifying a two-phase system. V

It is an important technique to obtain target products with higher yields by controlling the reaction and mass transfer. In this work, we focused on molecular weight control in the oxidative polymerization of phenol. We attempted selective production of phenol dimers through the formation of microdroplets in both single-and two-phase systems. In a single-phase system, selectivity of dimers to polymers can be improved by rapidly mixing ingredients using a micromixer. Further, we clarified the conditions to utilize such microspace effects by comparing the initial reaction time constant with the mixing time constant by order-of-magnitude estimation. In a two-phase system, it was clarified that controlling of mass transfer by formation of microdroplets using a micromixer was effective in the control of consecutive elementary reactions though the dimer selectivity hardly changes and the effect of micromixing was limited.