General procedure for the synthesis of 5. A 50 mL flask was charged with DT-TTF-(PhMeCOOEt) 4 (4) (100 mg, 0.10 mmol) and subjected to three cycles of evacuation and refilling with N 2 . Degassed MeOH (4 mL) and anhydrous THF (4 mL) were added to generate a suspension. In a separate flask, NaOH (50 mg, 1.1 mmol) was dissolved in degassed water (4 mL). The sodium hydroxide solution was added to 4 under nitrogen and the reaction was heated to reflux for 12 hours. The reaction was then cooled to room temperature and the volatiles were removed in vacuum. A 1M solution of HCl (5 mL) was added to afford an orange precipitate, which was collected by filtration and washed with water (20 mL) and CH 2 Cl 2 (20 mL). The product was collected and dried under vacuum for 12 hours to afford 5 as an orange solid (70 mg, 94 % yield). Characterisation: