1,5-二硝基萘的合成与分离纯化

Synthesis and Purification of 1,5-Dinitronaphthalene

报道了一种简单、温和、经济、有效的合成1,5-二硝基萘的新方法.首先以65%~68%的硝酸和较少量浓硫酸作硝化剂来替代高浓度的混酸硝化剂或其它复杂且使用不便的硝化剂,无需添加其它助剂及有机溶剂,在温和条件下能以94.4%的收率得到1,5-二硝基萘和1,8-二硝基萘的混合物.然后利用该混合物在丙酮中溶解性的差异,通过调控丙酮的用量及温度可方便地将1,5-二硝基萘进行分离纯化,收率可达42.3%.

A simple, mild, economical and efficient approach to 1, 5 - dinitronaphthalene is reported. Firstly, with 65% -68% nitric acid and a smaller amount of concentrated sulfuric acid as nitrating agent instead of concentrated nitrating agent of the mixed acid mixture or other complex and inconvenient nitrating agents, the mixture of 1, 5 - dinitronaphthalene and 1 , 8~dinitronaphthalene could be obtained in 94. 4% yield under mild conditions in the absence of additives and organic solvents. Then, based on their difference of dissolubility in acetone, 1, 5 - dinitronaphthalene could be separated conveniently in 42. 3% yield by controlling the amount and temperature of acetone.