氯尼达明合成路线的研究

Study on Synthetical Route of Lonidamine

目的:选择适合工业化生产的氯尼达明合成路线。方法:以乙酰苯肼为起始原料,与水合氯醛、盐酸羟胺在硫酸钠水溶液中生成N乙酰氨基肟基乙酰苯胺,然后环合,水解生成1H吲唑3羧酸,再与2,4二氯氯苄反应生成氯尼达明。结果:所得产物经元素分析、红外光谱及核磁共振谱确证了结构。结论:此工艺路线生产成本低廉,反应条件温和,适于工业化生产。

Objective： To find out an economical way for synthesizing lonidamine on industrial production scale. Methods： Lonidamine was synthesized from acetylphenylhydrazine by the reaction with chloral hydrate, hydroxylamine hydrochloride and sodium sulphate to form N-acetylaminoisonitrosoacetanilide, which was subsequently hydrolyzed to form 1H-indazole-3-carboxylic acid after Beckmann rearrangement and ring closing reaction. 1H-indazole-3-carboxylic acid reacted further with 2, 4-dichlorobenzyl chloride to give the product lonidamine. Results： Structure of Lonidamine was confirmed by element analysis, IR and I HNMR. Conclusion： This method is economical and convenient for industrial production.