3-羟基-5-甲氧基吡啶合成工艺

The Synthesis of 3-hydroxy-5-methoxy Pyridine

3-羟基-5-甲氧基吡啶作为一种药物中间体,其合成工艺的研究具有一定价值。本文对比研究了以3,5-二溴吡啶和N-苄基甘氨酸乙酯为原料的4条3-羟基-5-甲氧基吡啶的合成路线。其中以3,5-二溴吡啶为原料经甲醚化、氮氧化、氨解、脱氮氧和重氮化水解的5步反应工艺较好地合成了3-羟基-5-甲氧基吡啶1,总收率达到66. 7%。目标化合物结构经1H NMR、IR、MS和X-ray单晶衍射确证。该工艺操作简单,收率理想,可为目标产品工业化生产提供参考。

3-hydroxyl-5-methoxyl pyridine is an important intermediate of drug.It is valuable to research the synthetic process.In this paper,four synthesis routes of 3-hydroxyl-5-methoxyl pyridine,which used 3,5-dibromopyridine and N-benzyl glycine ethyl ester as raw materials,were studied.Among them,the 3-hydroxyl-5-methoxyl pyridine was successfully synthesized by the five step reaction process of methyletherification,nitrogen oxidation,aminolysis,denitrification and nitrification and hydrolysis 3,5-dibromopyridine was used as raw material with a total yield of 66.7%.The structure of aim compound was characterized by 1H NMR,IR,MS and X-ray single crystal.This synthesis method is simple with an ideal yield.It can provide reference for the industrial production of aim products.