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。
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
出处
《齐鲁药事》
2012年第3期132-133,共2页
qilu pharmaceutical affairs
