Synthesis
3-Fluorophenol (10 g, 89 mmol) was dissolved in acetic anhydride (90 mmol). Concentrated sulfuric acid (3 drops) was added as a catalyst and the reaction mixture was heated to 120°C. After completion of the reaction, the mixture was slowly poured into ice water (100 ml) containing NaHCO3 (1 g) to neutralize the acid. Subsequently, the organic phase was separated by extraction with ethyl acetate. The organic phase was washed sequentially with saturated NaHCO3 solution to remove residual acid and dried with anhydrous Na2SO4. Finally, the solvent was removed by distillation under reduced pressure to give 3-fluorophenol acetate (10.5 g), and the product was used directly in the subsequent reaction.
References
[1] Chemistry - A European Journal, 2015, vol. 21, # 5, p. 2241 - 2249
[2] Journal of Medicinal Chemistry, 1987, vol. 30, # 5, p. 814 - 820
[3] Journal of Medicinal Chemistry, 2018, vol. 61, # 7, p. 3037 - 3058
[4] Patent: CN105085427, 2018, B. Location in patent: Paragraph 0331; 0333; 0335; 0336