| 来氟米特合成工艺的改进 |
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| 引用本文： | 苏国栋,姜永悦,吕延文. 来氟米特合成工艺的改进[J]. 化工时刊, 2011, 25(4): 11-14. DOI: 10.3969/j.issn.1002-154X.2011.04.004 |
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| 作者姓名： | 苏国栋 姜永悦 吕延文 |
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| 作者单位： | 1. 衢州学院化学与材料工程学院,浙江,衢州,324000
2. 上海化工研究院,上海,200062 |
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| 摘 要： | 以乙酰乙酸乙酯与原甲酸三乙酯为原料,经缩合、环合得中间体5-甲基-4-异噁唑甲酸乙酯,不精馏直接将其碱水解15 min生成5-甲基-4-异噁唑甲酸,三步收率高达63.8%;再经氯化,不精制直接与对三氟甲基苯胺在乙酸乙酯溶剂中反应生成来氟米特粗品,粗品以乙酸乙酯为溶剂进行精制得高品质产品,经HPLC测量产品含量达99.9...
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| 关 键 词： | 来氟米特 乙酰乙酸乙酯 原甲酸三乙酯 合成 改进 |
Improvement in Synthesizing Technology of Leflunomide |
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| Su Guodong,Jiang Yongyue,Lv Yanwen. Improvement in Synthesizing Technology of Leflunomide[J]. Chemical Industry Times, 2011, 25(4): 11-14. DOI: 10.3969/j.issn.1002-154X.2011.04.004 |
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| Authors: | Su Guodong Jiang Yongyue Lv Yanwen |
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| Affiliation: | Su Guodong Jiang Yongyue Lv Yanwen(College of Chemical and Material Engineering,Quzhou University,Zhejiang Quzhou 324000;Shanghai Research Institute of Chemical Industry,Shanghai 200062) |
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| Abstract: | 5-Methylisoxazole-4-carboxylic acid ethyl ester,a drug intermediate of leflunomide,was synthesized from ethyl acetoacetate and triethoxy methane from ate by condensation and cyclization,and the ester was hydrolyzed by alkali without rectify to 5-Methylisoxazole-4-carboxylic acid,the yield was 63.8%;The acyl chloride of the acid reacted with p-trifluorom ethylaniline to leflunomide,the crude product was refined by acetic ether to high quality leflunomide,which content is 99.97%,and the content of isomer was less than 0.01%;The total yield was 41.0%,and improved 8.7%.At the same time,the mole ratio was optimized,the reaction was shorted,the synthesis was more safe and more Environment Protection,and the cost was lower. |
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| Keywords: | Leflunomide ethyl acetoacetate triethoxy methane synthesis improvement |
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