With the desired crosslinked frameworks in hand, we next sought to cleave the carbamate linkage and reveal exposed amine pairs. The thermal cleavage of tertiary carbamates has been successfully demonstrated not only in simple organic compounds but also in solid-state porous materials including silica and metalorganic frameworks. Thermogravimetric analyses confirmed the thermal sensitivity of the crosslinkers (Fig. ). Excitingly, subjecting 1-XL-18% to microwave heating at 230 °C in a mixture of 2-ethyl-1hexanol and ethylene glycol for 10 minutes resulted in quantitative carbamate cleavage and formation of 1-NH2-18%, a framework containing templated arylamines (Fig. ). No loss in crystallinity was detected by powder X-ray diffraction (PXRD) (Fig. ), and a large increase in the BET surface area from 2370 m 2 /g to 2650 m 2 /g was observed (Fig. ). This value is very close to the reported surface area for unfunctionalized Mg2dotpdc (~2700 m 2 /g). Full crosslinker removal was further confirmed by digestion 1 H NMR. No peaks associated with the crosslinker could be detected, and the amount of H4dotpdc-NH2 found was consistent with the starting amount of L1 (Fig. ).