To evaluate whether a wide range of building blocks and fuels can be used in the acylphosphate reaction cycle, we carried out a scope study. Since DMAP was found to be an efficient acylphosphate hydrolysis agent, it was used in combination with pyridine in the reaction cycles to facilitate hydrolysis within a reasonable amount of time. As figures of merit, we determined the activation yield after two minutes for the forward reaction, i.e., how much of the organophosphate was converted to the respective acylphosphate, and the hydrolysis half-life of the backward reaction. As can be seen in Figure and Table , the scope study included aromatic (1,2 and 5a-c), aliphatic ( ) and (poly-)phosphate-based (4, 6ab and 7ab) substrates. The overall conversion of the organophosphate substrate to the respective acylphosphate(s) proceeded in all cases nearly quantitatively. This finding suggests that the activation strategy applied herein can be used to acylate a wide range of organic phosphates. Furthermore, it is noteworthy that using 2-(phosphonooxy)benzoic acid as substrate intramolecular acylphosphate formation was achieved via transacetylation of acetic anhydride (compound 2). In the case of anhydride fuels other than acetic anhydride, for solubility reasons, the reactions had to be conducted in a 1:1 mixture of DMF/H2O (5a-c) and showed similar activation yields. Whereas the activation yields were comparable for the compounds shown, we observed pronounced differences in the hydrolysis half-lives.