| 2-甲基-5-甲氧基苯甲酸乙酯的合成工艺改进 |
| 投稿时间：2012-12-10 修订日期：2013-04-09 点此下载全文 |
| 引用本文：刘娜,魏海洋,武瑾,吕加国,朱驹,周有骏,郑灿辉.2-甲基-5-甲氧基苯甲酸乙酯的合成工艺改进[J].药学实践杂志,2013,31(5):377~379 |
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| 基金项目:国家自然科学基金(20972187). |
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| 中文摘要:目的 探索2-甲基-5-甲氧基苯甲酸乙酯的合成工艺改进方法。方法 以2-甲基-5-硝基苯甲酸为起始原料, 经酯化反应, 铁粉/醋酸还原, 重氮化水解反应, 甲基化反应等4步反应制得2-甲基-5-甲氧基苯甲酸乙酯。结果 还原反应中, 用廉价的铁粉/醋酸替代文献采用的昂贵的钯碳/氢气还原体系, 收率达95%;甲基化反应中, 以碳酸钾替代文献中的NaH, 收率达89.1%, 新合成工艺的收率由文献收率的63.21%提高到76.33%。结论 本方法提出了一条操作简便、条件温和、成本较低并适合放大制备的2-甲基-5-甲氧基苯甲酸乙酯的合成工艺路线。 |
| 中文关键词:2-甲基-5-硝基苯甲酸 2-甲基-5-甲氧基-苯甲酸乙酯 合成工艺 |
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| Improvement of the synthesis of 2-methyl-5-methoxy benzoic acid ethyl ester |
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| Abstract:Objective To improve the synthetic process of 2-methyl-5-methoxy benzoic acid ethyl ester. Methods The target compounds were prepared from 2-methyl-5-nitro-benzoic acid through esterification, reduction, diazotization hydrolysis and methylation.Results In the procedure of reduction, Pd/H2 system was replaced by Fe/AcOH with a yield of 92.7%. In the produce of methylation, potassium carbonate were used to take place of the NaH as deacid reagent with a yield of 89.1%. The yield of the new synthesis process was promoted from 75% to 89.1%. Conclusions This study provided a synthesis process route of 2-methyl-5-methoxy benzoic acid ethyl ester with simple operation, mild reaction condition, low price, which was suitable for the amplification of the preparation. |
| keywords:2-methyl-5-nitro-benzoic acid 2-methyl-5-methoxy benzoic acid ethyl ester synthesis |
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