3'-Bromoacetophenone/

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brief introduction

3' -bromoacetophenone, also known as m-bromoacetophenone, is an organic intermediate that can be synthesized from m-aminoacetophenone diazotization to form m-acetophenone diazo Chemicalbook hydrobromide by Sandmeyer reaction. 3' -bromoacetophenone can be used to prepare meptalol hydrochloride impurity D and 2-chloro-3 '-bromoacetophenone.

80ml48% hydrobromide, 80ml water and 23g m-aminoacetophenone were cooled with ice salt water to 0 ~ 5℃, and then a solution composed of 12.2g sodium nitrite and 30ml water (below the liquid level) was dropped under agitation, and the reaction temperature was maintained 0 ~ 8℃. After dropping, the reaction was continued for 30min. The prepared diazo salt solution was poured into cold CuBr hydrochloric acid solution (27.5gCuBr+50ml hydrobromic acid), heated to 50 ~ 65Chemicalbook℃, fully stirred and placed for 2 ~ 3h. Separation removes solid matter and water phase to produce oil. Wash the oil with water until the water solution is neutral. The oil is added to water and distilled with steam until there are no oil droplets. The oil layer was separated and the water layer was extracted with benzene. After merging the oil layer, the benzene was first evaporated under atmospheric pressure, and then the distillate at 117 ~ 122℃ (2.3kp) was collected by vacuum distillation to obtain 3' -bromoacetophenone (31.2g, 99.6%, 95.2% yield).

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