Please do not adjust margins Please do not adjust margins While performing DSC analysis of ADE prepared by thermomechanochemistry, we observed an endotherm prior to its melting point (Fig. ). More specifically, the presence of an endotherm peak around 112 °C (Fig. red), which appeared before melting endotherm at 144 °C, indicated a phase transition. In a repeated DSC experiment, we heated the starting compound to 115 °C, and powder X-ray diffraction (PXRD) analysis showed the appearance of a new crystalline phase (ESI Fig. ). When applying a different heating rate, we established a shift of the signal related to a polymorph transition (Fig. black), an indication of a kinetically irreversible phase transition. Additionally, in situ variabletemperature PXRD (VT-PXRD) measurements showed a phase transition between 100 °C and 110 °C (Fig. ), in excellent agreement with DSC results.