邻硝基苯乙酸合成工艺的改进  

Improvement of Synthetic Route of 2-Nitrophenylacetic Acid

作　　者：上官春轩[1] 王建龙[1] 张静[1] 常俊芳[1] 

机构地区：[1]中北大学,山西太原030051

出　　处：《上海化工》2010年第5期13-15,共3页Shanghai Chemical Industry

摘　　要：乙醇钠催化作用下使邻硝基甲苯与草酸二乙酯缩合,然后经水解、双氧水氧化、碳酸氢钠溶液萃取、过滤、盐酸酸化后得到邻硝基苯乙酸。通过改变工艺过程可以大大缩短合成时间,并且提高了产品纯度和得率。通过正交试验,得率由已报道的64%提高到87.84%。最佳反应条件为:邻硝基甲苯、乙醇钠、草酸二乙酯摩尔比为1∶1.2∶1.3,缩合温度为45℃,时间为3h,双氧水氧化温度为20℃以下。The o-nitrotoluene and diethyl oxalate are condensed under the catalysis of sodium ethoxide, then the o-bithophenylacetic acid was obtained through hydrogen peroxide’s hydrolysis and oxidation, sodium bicarbonate’s extraction and filtration, and the hydrochloride’s acidification. The condensation time can be shortened greatly through changing the process, and in the meantime improved the product purity. The condition of gaining the highest acquiring rate can be got through orthogonal test, furthermore the acquiring rate improves from the 64% reported to 87.84%.The optimal reaction conditions for synthesizing are as follows： o-nitrotoluene to sodium ethoxide and diethyl oxalate molar ratio of 1∶1.2∶1.28, condensation reaction ternperature of 50℃, condensation reaction time of 2.5h, oxidation reaction ternperature is lower than 20℃.

关 键 词：邻硝基苯乙酸 合成 邻硝基甲苯 有机中间体 

分 类 号：TQ246.16[化学工程—有机化工]