摘要
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。
ω,ω-Dibromo-p-phenyl acetophenone was synthesized from biphenyl,acetyl chloride and bromine.Firstly the reaction of biphenyl and acetyl chloride gave the p-phenyl acetophenone and its yield was close to 88.0%.Then,ω,ω-dibromo-p-phenyl acetophenone was obtained by bromination by the reaction of p-phenyl acetophenone using ethanol as the reaction medium.The effects of the reaction material ratio,temperature and time on the yield of the product were investigated.The optimal reaction conditions were obtained: ratio of bromine to p-phenyl acetophenone 2.2∶1,the reaction temperature ranges from 45~50 ℃ the reaction time 2.5 h.The yield under this optimum reaction conditions was up to 89.7%.m.p.114~116 ℃.The structure of the target product was confirmed by elementary analysis,FTIR and 1HNMR.The experimental results provide the important basic data for the industrial development of this product.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2010年第1期93-96,共4页
Fine Chemicals
基金
国家自然科学基金项目(20772096)~~