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合成邻硝基苯乙酸的最佳工艺

Optimum Synthetic Technical Investigation on o-Nitrophenylacetic Acid

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【作者】 李长恭邓月娥祝勇刘琳

【Author】 LI Chang-Gong DENG Yue-E ZHU Yong LIU Lin(School of Chemistry and Chemical Engineering,Henan Institute of Science and Technology,Xinxiang,Henan 453003,P.R.China)

【机构】 河南科技学院化学化工学院

【摘要】 在乙醇钠作用下邻硝基甲苯与草酸二乙酯缩合,再经水解、双氧水氧化、盐酸酸化合成邻硝基苯乙酸。本文针对邻硝基甲苯和草酸二乙酯的摩尔比、缩合反应时间、双氧水氧化温度等影响产率的关键变量进行正交试验,以产率为指标,研究合成邻硝基苯乙酸的最佳工艺条件:邻硝基甲苯与草酸二乙酯摩尔比1:1.3,温度50℃,缩合反应时间为2.5h,双氧水氧化温度10—20℃。

【Abstract】 o-Nitrotoluene condensed with diethyl oxalate under sodium ethoxide,and then the products synthetized o-nitroophenylacetic acid by the reactions of hydrolysis,oxidation by hydrogen peroxide,acidification by hydrochloric.The reaction conditions were optimized by orthogonal tests,and effects of investigation factors including the mole ratio of o-nitrotoluene to diethyl oxalate,condensation reaction time and oxidation temperature of hydrogen peroxide on the key variables of yield with yield as index,and the optimal synthetic conditions for o-nitroophenylacetic acid as follows: the molar ratio of o-nitrotoluene to diethyl oxalate was 1∶1.3,condensation reaction time was 2.5h,condensation temperature was 50℃ and oxidation temperature of hydrogen peroxide was 10—20℃.

【基金】 国家自然科学基金面上项目(21072046);河南科技学院高学历人才资助项目(08009)
  • 【文献出处】 光谱实验室 ,Chinese Journal of Spectroscopy Laboratory , 编辑部邮箱 ,2012年06期
  • 【分类号】TQ245
  • 【被引频次】1
  • 【下载频次】123
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