首页> 外国专利> NOVEL PREPARATION OF 1,8-DINITRONAPHTHALENE-3,6-DISULFONIC ACID, AND PREPARATION OF HIGH-PURITY 1-AMINO-8- HYDROXYNAPHTHALENE-3,6-DISULFONIC ACID USING ITS METHOD

NOVEL PREPARATION OF 1,8-DINITRONAPHTHALENE-3,6-DISULFONIC ACID, AND PREPARATION OF HIGH-PURITY 1-AMINO-8- HYDROXYNAPHTHALENE-3,6-DISULFONIC ACID USING ITS METHOD

机译:1,8-二硝基萘-3,6-二磺酸的新制备方法和高纯度1-氨基-8-羟基萘-3,6-二磺酸的制备方法

摘要

PURPOSE:To obtain the titled compound useful as an intermediate for dye in high yield, by dinitrating 2,7-naphthalenedisulfonic acid under specific conditions to give a high-purity compound, reducing and hydrolyzing it under specified conditions. CONSTITUTION:In nitrating 2,7-naphthalenedisulfonic acid with a mixed acid in a solvent of sulfuric acid, a reaction from a mononitro derivative to a dinitro derivative is carried out in conditions of reaction system wherein the dehydration value is 5-27, the reaction temperature is -20-40 deg.C, 6-15mol sulfuric acid is used based on 1mol naphthalene skeleton. After dropping of a nitrating agent is over, and no mononitro derivative is detected, the dinitro derivative is added to water, it is aged in a state of 80wt% sulfuric acid concentration for =0.5hr under heating (preferable 50 deg.C- the boiling point) to finish dinitration. 1,8-Dinitronaphthalene-3,6-disulfonic acid obtained by the dinitration is reduced with iron powder, and hydrolyzed to give 1-amino-8-hydroxynaphthalene-3,6- disulfonic acid.
机译:目的:通过在特定条件下将2,7-萘二磺酸进行硝化反应,以制得高纯度化合物,并在特定条件下将其还原和水解,从而以高收率获得用作染料中间体的标题化合物。组成:在硫酸溶剂中用混合酸硝化2,7-萘二磺酸时,在脱水值为5-27的反应体系条件下,由单硝基衍生物转化为二硝基衍生物。温度为-20-40℃,基于1mol萘骨架使用6-15mol硫酸。硝化剂滴加结束后,未检测到一硝基衍生物,将二硝基衍生物加入水中,在80wt%硫酸浓度的状态下加热(> 50hr-C进行老化> = 0.5hr)。沸点)以完成硝化反应。将通过该硝化而得到的1,8-二硝基萘-3,6-二磺酸用铁粉还原,进行水解而得到1-氨基-8-羟基萘-3,6-二磺酸。

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