4-正丁基-2-硝基苯胺的制备

以对正丁基苯胺为原料,合成了4-正丁基-2-硝基苯胺。经过酰化,硝化,水解等三步反应,总收率可达76%。其中酰化和硝化还可以合并成一锅法反应。用醋酐进行乙酰化反应,再用浓硝酸硝化,加入醋酐做溶剂。硝化结束后,用乙醇作溶剂经碱性水解得到目标产物。实验得出物料的优惠配比为:n(对正丁基苯胺)∶n(乙酸酐)=1∶3,n(对正丁基乙酰苯胺)∶n(醋酐)∶n(浓硝酸)=1∶3∶5,n(邻硝基对正丁基乙酰苯胺)∶n(氢氧化钾)=1∶1.3。

Synthesis of 4-Butyl-2-nitroaniline

4-Butyl-2-niroaniline was prepared from p-n-butylaniline through acylation,nitration and hydrolysis,and its total yield was 76 %. Among them,the acylation and nitration could be combined into one-pot reactor. The coumpound p,n-butylacetylaniline was got using the p,n-butylaniline and aceticanhydride as material. Acetic anhydride was used as solvent in the process of nitration. After that,the nitrification product was treated with alkaline hydrolysis using alcohol as solvent. The optimum ratios of reactants determined by experiments were n(p,n-butyl aniline) ∶ n(acetic anhydride)=1 ∶ 3,n(4-butylacetanilide)∶ n(acetic anhydride)∶ n(nitric acid)=1 ∶ 3 ∶ 5,n(p,n-butyl-acetylaniline) ∶ n(potassium hydroxide)=1 ∶ 1.3.