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Layered Ti3C2Tx MXene has been successfully intercalated and exfoliated with the simultaneous generation of a 3D silica network by treating its cationic surfactant intercalation compound (MXene-CTAB) with an alkoxysilane (TMOS), resulting in a MXene–silica nanoarchitecture, which has high porosity and specific surface area, together with the intrinsic properties of MXene (e.g., photothermal response). The ability of these innovative MXene silica materials to induce thermal activation reactions of previously adsorbed compounds is demonstrated here using NIR laser irradiation. For this purpose, the pinacol rearrangement reaction has been selected as a first model example, testing the effectiveness of NIR laser-assisted photothermal irradiation in these processes. This work shows that Ti3C2Tx-based nanoarchitectures open new avenues for applications that rely on the combined properties inherent to their integrated nanocomponents, which could be extended to the broader MXene family. [ABSTRACT FROM AUTHOR]