Reaction of Acetylenedicarboxylic Acid Made Easy: High-Pressure Route for Polymerization

A breakthrough has been achieved in improving the efficiency of solid-state polymerization of acetylenedicarboxylic acid (ADCA). Traditional solid-state polymerization of ADCA is marked by long exposure times of γ-radiation (>10 days) and very low yields (around 5.5%). We have been able to perform a reaction to an <i>n</i> = 8 oligomer, as confirmed by matrix-assisted laser desorption/ionization-time of flight, in less than 2 min by employing ∼6 GPa of pressure. We have determined the crystal structure of ADCA on increasing pressure to (5.2 GPa) to provide insight into the process of polymerization with Pixel calculations supporting our evaluation of the polymerization process