摘要
以市场易得的4-苯基环己酮为原料,经过与盐酸羟胺缩合得到4-苯基环己酮肟1;再在多聚磷酸作为酸催化剂以及反应溶剂的条件下发生Beckmann重排反应得到4-苯基己内酰胺2;最后用铝锂氢Li Al H4还原酰胺键得到4-苯基环庚胺3,三步反应平均收率为96.3%,总收率为89.4%。该方法具有原料易得,操作简便,产物收率高等优点,可推广合成至该类其它的取代环庚胺衍生物。
Starting from 4-phenylcyclohexanone, 4-phenyl cyclohexanone oxime 1 was obtained through condensation with hydroxylamine hydrochloride, then 4-phenylcycloheptanamide 2 was formed through Beckmann Rearrangement in the catalyst and solvent of polyphosphoric acid PPA. 4-phenylcycloheptanamine 3 was finally obtained by reduction with Li Al H4. The average yield of the three-step reaction was 96.3% and the total yield reached 89.4%. The preparation method has advantages of easy availability of raw materials, simple operation and high yield of the product, and can be applied the other substituted cycloheptanamine derivatives.
作者
王先恒
赵长阔
袁智
黄梅
WANG Xian-heng;ZHAO Chang-kuo;YUAN Zhi;HUANG Mei(School of Pharmacy,Zunyi Medical University,Zunyi,Guizhou 563000,Chin)
出处
《浙江化工》
CAS
2018年第7期12-15,共4页
Zhejiang Chemical Industry
基金
贵州省科技计划项目(黔科合SY[2015]3030)
遵义医学院自然科学类招标课题([2013]F-680)
