| 6-甲氧基靛红的合成工艺改进 |
| 投稿时间：2014-02-24 修订日期：2014-09-10 点此下载全文 |
| 引用本文：王鸿玉,宋云龙,章玲,曾强,朱驹,张辉.6-甲氧基靛红的合成工艺改进[J].药学实践杂志,2015,33(2):127~130 |
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| 基金项目:国家自然科学基金项目(81172928,21102174) |
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| 中文摘要:目的 探索6-甲氧基靛红的合成工艺改进方法。 方法 以3-甲氧基苯胺为起始原料,经Sandmeyer方法首先生成中间体1-肟基-N-(3-甲氧基苯基)乙酰胺,在甲磺酸催化下关环得到6-甲氧基靛红。 结果 在关环反应中,催化剂采用甲磺酸,替代文献中常用的浓硫酸,温度80℃,反应30 min,收率达81.24%。 结论 提出了一条操作简单、条件温和、收率高的6-甲氧基靛红的合成工艺,适合大量制备。 |
| 中文关键词:6-甲氧基靛红 合成工艺 甲磺酸 |
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| Improvement of synthesis method of 6-methoxyisatin |
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| Abstract:Objective To improve the synthetic condition of 6-methoxyisatin. Methods The starting material 3-methoxyaniline was firstly converted into the intermediate 1-oximino-N- (3-methoxyphenyl) acetamide through Sandmeyer reaction, then 6-methoxyisatin was conducted with methanesulfonic acid as catalyst in the following ring closure reaction. Results In the second step of the cyclization reaction, methanesulfonic acid was used to replace the concentrated sulfuric acid which is widely used in literature. The temperature was 80℃, the reaction time was 30 min, and the yield was 81.24%. Conclusion This study provided a synthesis process of 6-methoxyisatin with simple operation, mild reaction condition and high yield, which is suitable for large scale preparation of the compound. |
| keywords:6-methoxyisatin synthesis methanesulfonic acid |
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