At room temperature, 0.28 g (0.003 mol) of phenol, 1.7 g (0.03 mol) of potassium hydroxide (KOH), an appropriate amount of water, and dioxane were added as solvents to a 50 mL round bottom flask. The reaction mixture was heated to 50°C, followed by the passage of trifluoromethane gas bubbling through the reaction solution for 2 hours. After completion of the reaction, the mixture was stirred at 50 °C overnight. The yield of difluoromethoxybenzene was calculated to be 70% by 19F NMR analysis (Figures 1 and 2 show the 19F NMR decoupling and proton coupling spectra of the reaction mixture and the purified difluoromethoxybenzene, respectively), using the 19F NMR integral signal of the HF2CO group as an internal standard.
