Synthesis
80ml of 48% hydrobromic acid, 80ml of water and 23g m-amino acetophenone, with ice brine cold to 0 ~ 5 C, and then drop under stirring by 12.2g of sodium nitrite and 30ml of water solution (under the liquid level), and maintain the reaction temperature of 0 ~ 8 C. Drops, and continue to react for 30min. will be made above the diazonium salt solution is poured into the cold CuBr hydrochloric acid solution (27.5 gCuBr + 50 ml hydrobromic acid), heated to 50 ~ 65 , stirred thoroughly for 2 ~ 3h. Separate and remove the solid material and water phase, to obtain the oily material. The oily material was washed with water until the aqueous solution was neutral. The oily material was added to water and distilled with water vapor until there were no oil droplets. Separate the oil layer, the aqueous layer was extracted with benzene, and after combining the oil layers, the benzene was first vaporized at atmospheric pressure, and then distilled at reduced pressure to collect the fraction at 117-122C (2.3 kp), to obtain the product 3'-bromoacetophenone (31.2g, content 99.6%, yield 95.2%).
