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Human-in-the-loop experimentation enables interactive machine learning for continuous flow chemistry reaction planning and optimization. 

ABSTRACT A series of Diels–Alder (DA) crosslinked polymethacrylate networks covering a broad range of glass‐transition temperatures (T_g) was prepared to establish the relationship between theT_gand the thermal decrosslinking behavior of these networks. A series of permanently crosslinked and uncrosslinked analogues were also prepared to better understand the thermoset‐to‐thermoplastic transition occurring in the DA networks at elevated temperatures. The network series were studied using dynamic mechanical analysis, which established an inverse relationship betweenT_gand decrosslinking ability. Differential scanning calorimetry confirmed the viability of the DA linkages in all formulations, and a trapping experiment with 9‐anthracenemethanol demonstrated that even the least responsive network was capable of undergoing decrosslinking given appropriate thermal treatment. While polymer chain mobility has long been understood to be a critical factor in healable materials, this work verifies the importance of this parameter in the decrosslinking of DA networks. © 2019 Wiley Periodicals, Inc. J. Polym. Sci.2020,58, 193–203