山东化工
山東化工
산동화공
SHANDONG CHEMICAL INDUSTRY
2014年
9期
13-15
,共3页
颉林%王守伟%赵立祥%郑晓明
頡林%王守偉%趙立祥%鄭曉明
힐림%왕수위%조립상%정효명
2 - 羟基吡啶%2 - 氨基吡啶%重氮化%水解
2 - 羥基吡啶%2 - 氨基吡啶%重氮化%水解
2 - 간기필정%2 - 안기필정%중담화%수해
2 - hydroxypyridine%2 - aminopyridine%diazotization%hydrolysis
以2-氨基吡啶为原料,在20%(质量分数)的硫酸溶液中,通过滴加过量的10%(质量分数)的亚硝酸钠,在0~5℃左右进行重氮化反应,重氮液在 Na2 CO3溶液中水解、中和后合成2-羟基吡啶,采用结晶和重结晶的方法,得到含量为98%以上的2-羟基吡啶,产物收率可达78%左右。本方法设计的合成路线步骤简单、反应时间短、易于操作和适合工业化。
以2-氨基吡啶為原料,在20%(質量分數)的硫痠溶液中,通過滴加過量的10%(質量分數)的亞硝痠鈉,在0~5℃左右進行重氮化反應,重氮液在 Na2 CO3溶液中水解、中和後閤成2-羥基吡啶,採用結晶和重結晶的方法,得到含量為98%以上的2-羥基吡啶,產物收率可達78%左右。本方法設計的閤成路線步驟簡單、反應時間短、易于操作和適閤工業化。
이2-안기필정위원료,재20%(질량분수)적류산용액중,통과적가과량적10%(질량분수)적아초산납,재0~5℃좌우진행중담화반응,중담액재 Na2 CO3용액중수해、중화후합성2-간기필정,채용결정화중결정적방법,득도함량위98%이상적2-간기필정,산물수솔가체78%좌우。본방법설계적합성로선보취간단、반응시간단、역우조작화괄합공업화。
2 - Hydroxypyridine was prepared by diazotization of 2 - aminopyridine,dissoving in 20% sulfuric acid solution and putting NaNO2 solution in excess of about 10% into the solution. The appropriate temperature of diazotization is 0 ~5℃ ,followed by an alkaline hydrolysis process in Na2 CO3 solution. Thus,2 - hydroxypyridine was gained together with sodium sulfate. To purify the 2 - hydroxypyridine needs methods of crystallization and recrystallization for extraction. At last high quality of 2 - hydroxypyridine was synthesized with 98% content. And the yield could be satisfied as high as 78%or so. The time needed by the route is much shorter than that of the references,and has simpler operation than others. The process is very suitable for industrial.