Apart from the DTO degradation product and residual pDOT, only minor other signals were observed in the 1 H NMR spectrum, Figure . SEC analysis (Figure ) showed shifts toward lower observed molar masses, indicating the partial degradation of chains, as is common for a controlled depolymerization. For comparison, a sample of MeOTf-initiated pDOT was heated to 140 °C in DMF. Faster thermal degradation was observed with 67 mol-% DTO formed after 20 h (Figure , Table , entry 3) together with a large shift in SEC-measured molar mass (Figure ). With continuing heating, the sample degraded fully into small molecules after 3 days (Figure ), but NMR analysis (Figure ) showed the formation of multiple side products.