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苯乙酮酸乙酯的合成工艺研究
Study on the Synthesis Process of Ethyl Phenyl Glyoxylate
【摘要】 苯与草酸单乙酯酰氯在无水三氯化铝的催化作用下合成苯乙酮酸乙酯,工艺最佳条件为:n(草酸单乙酯酰氯)=0.18 mol,n(苯)∶n(三氯化铝)∶n(草酸单乙酯酰氯)=6∶1.3∶1,反应温度为20~25℃,反应时间为3 h,苯乙酮酸乙酯产率达96.21%,采用减压蒸馏可使产物纯度达95.58%.其产物结构经1HNMR、红外光谱、紫外光谱表征.
【Abstract】 Ethyl phenyl glyoxylate is synthesised from benzene and ethyl chloride glyoxylate with anhydrous aluminum trichloride as the catalyst.The optimum conditions for the reaction are obtained as follows: n(ethyl chloride glyoxylate) =0.18 mol,the molar ratio of benzene to aluminum trichloride to ethyl chloride glyoxylate 6:1.3:1,reaction temperature 20~25 ℃,reaction time 3 h.The yield is 96.21 %,and the purity is 95.58 %(HPLC) by vacuum distillation.The structure of ethyl phenyl glyoxylate is confirmed by 1HNMR,IR,UV spectra.
【关键词】 苯乙酮酸乙酯;
草酸单乙酯酰氯;
傅氏酰基化反应;
【Key words】 ethyl phenyl glyoxylate; synthesis; process improvement;
【Key words】 ethyl phenyl glyoxylate; synthesis; process improvement;
- 【文献出处】 江西理工大学学报 ,Journal of Jiangxi University of Science and Technology , 编辑部邮箱 ,2011年01期
- 【分类号】TQ245.24
- 【被引频次】8
- 【下载频次】269