| 吉美嘧啶及其关键中间体的制备 |
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| 引用本文： | 马玉贞,张广洲.吉美嘧啶及其关键中间体的制备[J].齐鲁药事,2012,31(3):132-133. |
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| 作者姓名： | 马玉贞 张广洲 |
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| 作者单位： | 1. 山东商业职业技术学院生物工程学院,山东,济南,250103
2. 山东省医药工业研究所,山东省化学药物重点实验室,山东,济南,250101 |
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| 摘 要： | 目的经过工艺改进摸索精制吉美嘧啶及其关键中间体5-氯-3-氰基-4-甲氧基-2(1 H)吡啶酮的方法。方法以丙二腈、原乙酸三甲酯及1,1-二甲氧基三甲胺为起始原料,经过缩合、闭环、氯代及水解等一系列反应,制备替吉奥有效成分吉美嘧啶。结果精制后的中间体纯度在99.8%以上,单杂控制在0.1%以下。结论用精制后的中间体制备出吉美嘧啶,纯度在99.9%以上,总收率45%。此工艺成本低,容易操作,且适合工业化生产。
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| 关 键 词： | 吉美嘧啶 5-氯-4-羟基-2(1H)吡啶酮 中间体 |
The synthesis of gimeracil and its key intermediate |
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| MA Yu-zhen
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ZHANG Guang-zhou.The synthesis of gimeracil and its key intermediate[J].qilu pharmaceutical affairs,2012,31(3):132-133. |
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| Authors: | MA Yu-zhen ZHANG Guang-zhou |
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| Institution: | 1. Biotechnology Department ,Shandong Institute of Commerce and Technology,Jinan 250103 ;2. Shandong Institute of Pharmaceutical Industry, Shandong Provincial Key Laboratory of Chemical Drug, Jinan 250101 , China ) |
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| Abstract: | Objective To grope a new method for the purification of gimeracil and its key intermediate 5 - chloro - 4 - hy- droxy - 2 -（ 1H ） - pyridone by improvement of technology. Methods The gimeracil was prepared from the raw materials mal- ononitrile, trimethyl orthoacetate and N, N - imethylfirmanmide dimethyl acetal by the reactions of condensation, cyclization, chlorination and hydrolysis. Results The purity of the intermediate was higher than 99.8% and the single impurity was lower than 0.1%. Conclusion The purity of the gimeracil was above 99.9% and the total yield was 45%. The process was low cost, easy operate and suitable for industrialized production |
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| Keywords: | Gimeracil 5 - chloro - 4 - hydroxy - 2 - （ 1H ） - pyridinone Intermediate |
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