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以联苯、乙酰氯、溴素为原料,合成了ω,ω-二溴对苯基苯乙酮。首先,联苯和乙酰氯反应生成对苯基苯乙酮,收率88.0%;然后,对苯基苯乙酮以乙醇为反应介质,经溴素溴化合成ω,ω-二溴对苯基苯乙酮。重点探讨了溴化过程中原料摩尔比、反应温度、反应时间等因素对反应收率的影响。最佳反应条件为:n(溴素)∶n(对苯基苯乙酮)=2.2∶1,反应温度45~50℃,反应时间2.5 h,总收率达89.7%。产物熔点114~116℃。用元素分析、傅立叶变换红外光谱(FTIR)和核磁共振氢谱(1HNMR)确定了目标化合物的结构。研究结果为工业开发实验提供了依据。
Using biphenyl, acetyl chloride and bromine as raw materials, ω, ω-dibromo-p-phenylacetophenone was synthesized. First, biphenyl and acetyl chloride generated p-phenylacetophenone, the yield of 88.0%; then, p-phenyl acetophenone to ethanol as the reaction medium, bromine bromine synthesis of ω, ω-dibromo-phenyl Acetophenone. The effects of molar ratio of raw materials, reaction temperature and reaction time on the yield of the reaction were discussed. The optimal reaction conditions were as follows: n (bromine): n (p - phenylacetophenone) = 2.2:1, reaction temperature 45 ~ 50 ℃, reaction time 2.5 h, total yield 89.7%. The product m.p. 114-116 ° C. The structure of the target compound was confirmed by elemental analysis, Fourier transform infrared spectroscopy (FTIR) and 1H nuclear magnetic resonance (1HNMR). The results provide the basis for industrial development experiment.