以2-甲基萘（2-MN）为原料，冰醋酸为溶剂，（NH₄）₂S₂O₈为引发剂，经30% H₂O₂氧化制得粗品2-甲基-1，4-萘醌（2-MNQ），通过IR、NMR、MS对其结构进行表征，并采用HPLC （面积归一化法）测定粗品2-MNQ的纯度及其所含杂质的种类和含量。考察了反应温度、反应时间、溶剂与氧化剂用量对粗品2-MNQ收率、纯度、转化率的影响，并得到最佳工艺条件：反应温度为85℃、反应时间为3 h、n（CH₃COOH）∶n（H₂O₂）∶n（2-MN）=50∶11∶1。在最佳工艺条件下，粗品收率为61.1%，转化率为99.7%，纯度为87.7%。经HPLC法测得粗品2-MNQ中的杂质主要为邻苯二甲酸酐和6-甲基-1，4-萘醌（6-MNQ），粗品依次经NaHCO₃水溶液和NaHSO₃水溶液处理，最终获得2-MNQ纯品（纯度97.7%），总收率为56.2%。

Crude 2-methyl-1,4-naphthoquinone (2-MNQ) is prepared by using 2-methylnaphthalene (2-MN) as raw material,glacial acetic acid as solvent,30% H₂O₂ as oxidant and (NH₄)₂S₂O₈ as initiator.Its structure is confirmed by IR,NMR and MS spectra.The purity of crude product,and the type and content of impurities contained therein are determined by HPLC (area normalization method).The optimum process conditions are obtained through investigating the effects of reaction temperature,reaction time,amounts of solvent and oxidant on the yield,purity and conversion of crude 2-MNQ.The optimum reaction temperature is 85℃,the optimum reaction time is 3 h,and the optimum n(CH₃COOH)：n(H₂O₂)：n(2-MN) is 50：11：1.Under the optimum conditions,crude product yield can reach 61.1%,the conversion is 99.7%,and the purity is 87.7%.Through HPLC determination,crude 2-MNQ contains main impurities including phthalic anhydride and 6-methyl-1,4-naphthoquinone (6-MNQ).Pure 2-MNQ with a purity of 97.7% can be obtained by processing crude 2-MNQ with NaHCO₃ and NaHSO₃ aqueous solutions in turn,the total yield is 56.2%.

乔琼清(1994-),男,硕士研究生,主要从事有机合成与催化,qiaoliang940910@126.com