氮-氨基-3-氮杂双环[3.3.0]辛烷盐酸盐合成工艺研究  

Research on the preparation of nitrogen-amino-3-azabicyclo[3.3.0]octane hydrochloride

作　　者：江正祥 申红艳 李国防[2] 

机构地区：[1]上海现代哈森(商丘)药业有限公司,河南商丘476000 [2]商丘师范学院有机新材料合成重点实验室,河南商丘476000

出　　处：《应用化工》2010年第10期1495-1497,共3页Applied Chemical Industry

基　　金：河南省科技攻关资助(92102210121)

摘　　要：以3-氮杂双环[3.3.0]辛烷盐酸盐为原料,采用亚硝化和金属还原两步法与氯胺法制备氮-氨基-3-氮杂双环[3.3.0]辛烷盐酸盐,利用正交实验研究了工艺条件对产品收率的影响。实验说明,亚硝化和金属还原两步法适合工业化,亚硝化温度85℃,溶液pH值1.5,还原温度30℃,N-亚硝基-氮杂双环[3.3.0]辛烷被锌粉还原,氮-氨基-3-氮杂双环[3.3.0]辛烷盐酸盐的总收率大于90%。Using 3-azabicyclo[3.3.0]octane hydrochloride as starting materials,nitrogen-amino-3-azabicyclo[3.3.0]octane hydrochloride was prepared by nitrosation,metal reduction process and chloramine method.The influence of reaction conditions on the yield of the product was investigated by orthogonal experiment.The results showed that the nitrosation and metal reduction two-step process can be applied for industrialization.3-Azabicyclo[3.3.0]octane hydrochloride was nitrosatied firstly at 85 ℃ in pH 1.5 solution and then reduced to nitrogen-amino-3-azabicyclo[3.3.0]octane hydrochloride by Zn powder,and the total yield of the product was more than 90%.

关 键 词：氮-氨基-3-氮杂双环[3.3.0]辛烷盐酸盐 亚硝化 氯胺 

分 类 号：O624.4[理学—有机化学]