【摘要】 以对羟基苯甲醛为原料 ,首先与盐酸羟胺及甲酸钠在甲酸中反应合成对羟基苯甲腈 ,收率为 88.6% ,然后在冰醋酸中与浓硝酸反应合成出 3-硝基 - 4-羟基苯甲腈 ,收率为 92 .9% ,后者再与碘及过氧化氢在酸性乙醇溶液中反应合成出硝碘酚腈 ,收率为 93.9% ,总收率为 77.3%。通过元素分析、IR及 MS等手段对中间体及目标产物的结构进行了确证。该方法原料易得 ,操作简便 ,收率高。更多还原

【Abstract】 Nitroxynil was prepared from p hydroxybenzaldehyde by cyanation, nitration and iodination reactions. Firstly, p hydroxybenzonitrile was obtained in 88.6% yield by the reaction of p hydroxyben zaldehyde with hydroxylamine hydrochloride and sodium formate in formic acid; secondly, p hydroxyben zonitrile reacted with nitric acid in glacial acetic acid to give 92.9% 4 hydroxy 3 nitrobenzonitrile; and thirdly, the latter was iodinated directly with iodine in the presence of hydrogen peroxide to yield 93.9% nitroxynil(77.3% based on p hydroxybenzaldehyde). The structures of the intermediates and the title compound were identified with IR, MS and elemental analysis. The results showed that the method had a feature of lower cost and higher yield.更多还原