CN110963924A - 一种邻氯对硝基苯胺的制备方法 - Google Patents

一种邻氯对硝基苯胺的制备方法 Download PDF

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CN110963924A
CN110963924A CN201811153073.9A CN201811153073A CN110963924A CN 110963924 A CN110963924 A CN 110963924A CN 201811153073 A CN201811153073 A CN 201811153073A CN 110963924 A CN110963924 A CN 110963924A
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nitroaniline
chloro
solid
temperature
washing
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吴凯
黄焕军
严学文
伍重远
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
    • C07C209/74—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton by halogenation, hydrohalogenation, dehalogenation, or dehydrohalogenation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

本发明公开了一种邻氯对硝基苯胺的制备方法，将质量分数20%的盐酸溶液加入反应瓶中，升温至60℃后加入对硝基苯胺，保温搅拌至固体完全溶解后降至室温；反应液用冰盐降至‑3℃到3℃，缓慢滴加质量分数为5%的次氯酸钠溶液，反应6h后使用淀粉碘化钾试纸监测，当试纸变成微蓝色，过滤，固体用碱洗，水洗至中性，烘干得到邻氯对硝基苯胺；本发明工艺流程短、操作简单、原料来源广、副反应少产物纯度高，具有实际使用和推广价值。

Description

一种邻氯对硝基苯胺的制备方法
技术领域
本发明属于化合物合成技术领域，具体是一种邻氯对硝基苯胺的制备方法。
背景技术
邻氯对硝基苯胺是生产多种染料、颜料和医药的重要中间体，可以通过重氮化合成分散红玉2GFL、分散大红3GFL、分散红玉P-B、分散红S-BGL、分散大红SE-GFL、分散橙S2、分散大红2GFL等，还可以作为有机颜料耐晒艳黄10G、银朱R的重氮组成，也是冰染色基棕色盐V和阳离子红GTL及灭钉螺的农药——贝螺杀等的原料,用途十分广泛。目前产品呈膏状、含量低、运输、使用都不方便，关于邻氯对硝基苯胺合成工艺研究很多，但并不成熟，合成工艺指标需要进一步研究探索。
发明内容
本发明的目的就是提供一种操作简单、原料来源广、副反应少的邻氯对硝基苯胺的制备方法。
本发明包括以下步骤：（1）将质量分数20%的盐酸溶液加入反应瓶中，升温至60℃后加入对硝基苯胺，保温搅拌至固体完全溶解后降至室温；
（2）将（1）中的反应液用冰盐降至-3℃到3℃，缓慢滴加质量分数为5%的次氯酸钠溶液，反应6h后使用淀粉碘化钾试纸监测，当试纸变成微蓝色，过滤，固体用碱洗，水洗至中性，烘干得到邻氯对硝基苯胺。
本发明工艺流程短、操作简单、原料来源广、副反应少产物纯度高，具有实际使用和推广价值。
具体实施方式
本发明包括以下步骤：（1）将质量分数20%的盐酸溶液加入反应瓶中，升温至60℃后加入对硝基苯胺，保温搅拌至固体完全溶解后降至室温；
（2）将（1）中的反应液用冰盐降至-3℃到3℃，缓慢滴加质量分数为5%的次氯酸钠溶液，反应6h后使用淀粉碘化钾试纸监测，当试纸变成微蓝色，过滤，固体用碱洗，水洗至中性，烘干得到邻氯对硝基苯胺。

Claims (1)

1.一种邻氯对硝基苯胺的制备方法，其特征在于包括以下步骤：（1）将质量分数20%的盐酸溶液加入反应瓶中，升温至60℃后加入对硝基苯胺，保温搅拌至固体完全溶解后降至室温；
（2）将（1）中的反应液用冰盐降至-3℃到3℃，缓慢滴加质量分数为5%的次氯酸钠溶液，反应6h后使用淀粉碘化钾试纸监测，当试纸变成微蓝色，过滤，固体用碱洗，水洗至中性，烘干得到邻氯对硝基苯胺。
CN201811153073.9A 2018-09-30 2018-09-30 一种邻氯对硝基苯胺的制备方法 Pending CN110963924A (zh)

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CN201811153073.9A CN110963924A (zh) 2018-09-30 2018-09-30 一种邻氯对硝基苯胺的制备方法

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CN201811153073.9A CN110963924A (zh) 2018-09-30 2018-09-30 一种邻氯对硝基苯胺的制备方法

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CN110963924A true CN110963924A (zh) 2020-04-07

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Application publication date: 20200407