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环己醇在以浓硫酸和磷酸组成的混合酸催化作用下,脱水得到环己烯,且当混合酸中浓硫酸和磷酸的体积比为1∶2时,环己烯的收率最高;在乙二醇(EG)作用下,亚硝酸钠和碘在乙酸乙酯和水中硝化环己烯得到标题化合物,其结构经1HNMRI、R和元素分析表征。该“一锅”合成法采用碘-乙二醇/亚硝酸钠替代氯化汞/亚硝酸钠硝化环己烯制备标题化合物,不涉及用碱液对中间产物的处理,也避免了高毒性有机试剂的使用且反应为均相体系,预处理简单方便,产率较高。
Cyclohexanol was dehydrated to cyclohexene under the catalysis of mixed acid composed of concentrated sulfuric acid and phosphoric acid. The yield of cyclohexene was the highest when the volume ratio of concentrated sulfuric acid to phosphoric acid was 1: 2 in mixed acid. Ethylene glycol (EG), sodium nitrite and iodine nitration of cyclohexene in ethyl acetate and water to give the title compound, its structure by 1HNMRI, R and elemental analysis. The “one-pot” synthesis method uses iodine-ethylene glycol / sodium nitrite instead of mercuric chloride / sodium nitrite to nitration of cyclohexene to prepare the title compound without involving the treatment of the intermediate with lye and also avoiding high The use of toxic organic reagents and the reaction system is homogeneous, pretreatment is simple and convenient, high yield.