亚硫酸氢钠甲萘醌中间体2-甲基-1,4-萘醌的绿色合成

Green Synthesis of an Intermediate 2-methyl-1,4-naphthoquinone of Sodium Bisulfite Menadione

以2-甲基萘为原料合成了亚硫酸氢钠甲萘醌的中间体2-甲基-1,4-萘醌。使用过硫酸钾为引发剂,过氧化氢为氧化剂,乙酸为溶剂,探究了过硫酸钾与2-甲基萘的质量比、过氧化氢用量、反应温度、时间等单因素对合成中间体2-甲基-1,4-萘醌产率的影响。在单因素实验的基础上,进行正交实验,得到最佳合成条件:2-甲基萘1.42 g(0.01 mol)、过硫酸钾与2-甲基萘的质量比为3%、过氧化氢9.3 mL[即n(过氧化氢)∶n(2-甲基萘)为12∶1]、乙酸9.5 mL[即n(乙酸)∶n(2-甲基萘)为15∶1]、反应温度为80℃、反应时间为3 h,其产率达到55.9%。在优化合成工艺的同时,达到了既绿色环保又高效合成的目的。

The intermediate 2-methyl-1,4-naphthoquinone of sodium bisulfite menadione was synthesized from 2-methylnaphthalene.Using potassium persulfate as initiator,hydrogen peroxide as oxidant and acetic acid as solvent,the effects of the mass ratio of potassium persulfate to 2-methylnaphthalene,the amount of hydrogen peroxide,reaction temperature and time on the yield of 2-methyl-1,4-naphthoquinone were investigated.On the basis of single factor experiment,orthogonal experiment was carried out to obtain the optimal synthesis conditions as follows:2-methylnaphthalene 1.42 g(0.01 mol),the mass ratio of potassium persulfate to 2-methylnaphthalene is 3%,hydrogen peroxide 9.3 mL[n(hydrogen peroxide)∶n(2-methylnaphthalene)is 12∶1],acetic acid 9.5 mL[n(acetic acid)∶n(2-methylnaphthalene)is 15∶1],the reaction temperature is 80℃,the reaction time is 3 hours,the yield reaches 55.9%.At the same time of optimizing the synthesis process,the purpose of both green and efficient synthesis was achieved.