邻硝基苯胺的合成研究

Research of Synthesis of o-Nitroaniline

以苯胺为原料,经过冰醋酸酰化,混酸硝化、酸性条件下水解合成邻硝基苯胺。对影响该产物合成的因素进行了考察。结果表明:酰化最佳反应条件,分馏温度103℃左右,苯胺:冰醋酸:锌粉=0.1mol:0.23mol:0.1g;硝化反应反应温度控制在35℃,乙酰苯胺:冰醋酸:浓硫酸=0.03 mol:0.085 mol:0.112 mol,混酸:硫酸=0.05 mol:0.17mol;在酸性条件下水解:采用70%硫酸在空气浴的条件下,加热回流0.5 h至暗红色即可,产率为49.38%。该合成方法反应条件温和。

Using aniline as the material, through acetic acid acylation and mixed acid nitration, hydrolysis has been the product of o-Nitroaniline under acidic conditions. Factors that influence the synthesis of the product are researched. The results show that the best conditions for acylation reactions are ：fractionation temperature is around 103 ℃; the rate of glacial acetic acid aniline and zinc are 0. 1 mol： 0.23mol： 0. 1g, temperature of nitration is controlled at about 35℃, the rate of acetanilide ,glacial acetic acid and concentrated sulfuric acid are 0.03mol： 0.085mol： 0.112mol;rate of mixed acid and sulfuric acid are 0.05mol：0.17mol.Materials should be hydrolysis in acidic conditions. 70% sulfuric acid is heated dark red in 0.5h in air bath. The yield is about 49.38%. The condition of this synthetic methods is mild.