While there have been reports of separate tertiary carbamate or tertiary ester 23 thermolysis in metal-organic frameworks, prior to this work the simultaneous cleavage of both groups within a single framework was not known. Excitingly, upon microwave heating at 230 °C, the mixed tertiary ester/carbamate crosslinker in 1-crosslinked could be cleanly removed to generate 1templated, a framework containing acid and base pairs. Experimentally we have found that the primary amines in 1-templated have heightened oxidative sensitivity due to the presence of neighboring acidic groups, and the microwave reaction must be done using samples that have been rigorously sparged and sealed under N2.