Synthesis
Under argon protection, 1,3-dibromobenzene (4.1 g, 17.5 mmol) and anhydrous aluminum trichloride (5.6 g, 42 mmol) were placed in a 50 mL two-neck flask. Acetyl chloride (2.0 mL, 28 mmol) was slowly added dropwise at room temperature. After the dropwise addition, the reaction system was slowly heated to 100 °C, during which a large amount of hydrogen chloride gas was released. The reaction was maintained at this temperature for 1.5 hours. After completion of the reaction, the system was cooled to room temperature and slowly poured into a mixture of crushed ice and concentrated hydrochloric acid. The organic phase was separated and washed sequentially with water, sodium carbonate solution and brine. The organic phase was dried with anhydrous magnesium sulfate and evaporated under reduced pressure to remove the solvent. Finally, the target product 2',4'-dibromoacetophenone (4.5 g, 93% yield) was purified by column chromatography.
References
[1] Advanced Synthesis and Catalysis, 2016, vol. 358, # 6, p. 926 - 939
[2] Patent: CN106316958, 2017, A. Location in patent: Paragraph 0145; 0146; 0152; 0153
[3] Journal of the Chemical Society, 1949, p. 1133,1136
[4] Roczniki Chemii, 1973, vol. 47, p. 2333 - 2337
