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1-羟基环己基苯基甲酮合成新工艺研究

Study on a new process for synthesis of 1-Hydroxycyclohexyl phenyl methanone

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【作者】 丁成荣陈林青王友昌来虎钦

【Author】 DING Cheng-rong,CHEN Lin-qing,WANG You-chang,LAI Hu-qin(College of Chemical Engineering and Materials Science,Zhejinag University of Technology,Hangzhou 310032,China)

【机构】 浙江工业大学化学工程与材料学院

【摘要】 研究了以环己甲酸为起始原料,经酰化、傅克反应制得环己基苯基甲酮,再与氢氧化钠在四氯化碳及相转移催化剂的存在下反应生成1-羟基环己基苯基甲酮的新工艺.较佳反应条件是傅克反应温度为78℃,n(环己甲酰氯)∶n(三氯化铝)=1∶1.1,n(环己甲酰氯)∶n(苯)=1∶4,回流反应时间4 h;α羟基化反应时间为10 h.在较佳工艺条件下反应总收率达65%,纯度98.2%.1-羟基环己基苯基甲酮产品结构由IR1、H NMR确认.该过程所用原料较为廉价、操作简便,具有工业化应用前景.

【Abstract】 1-Hydroxycyclohexyl phenyl methanone was prepared from cyclohexane carboxylic acid by the reaction of acyl chloridation,Frield-Crafts reaction and α-hydroxylating with sodium hydroxide in the presence of carbon tetrachloride and PTC.The optimum reaction conditions were as follows: Frield-Crafts reaction temperature was 78 ℃,n(cyclohexyl carbonyl chloride)∶n(aluminum trichloride)=1∶1.1,n(cyclohexyl carbonyl chloride)∶n(benzene)=1∶4.The reflux time was 4 h.α-hydroxylating reaction time was 10 h.Under the optimal conditions,the overall yield of 1-Hydroxycyclohexyl phenyl methanone is 65% with the purity of 98.2%.The structure of 1-Hydroxycyclohexyl phenyl methanone was characterized by IR and 1H NMR.The advantages of the above synthetic process are easy operation,cheap raw materials.So it can be considered of a good prospect for the industrial application.

  • 【文献出处】 浙江工业大学学报 ,Journal of Zhejiang University of Technology , 编辑部邮箱 ,2009年03期
  • 【分类号】TQ244.2
  • 【被引频次】3
  • 【下载频次】619
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