9-苄基-9-氮杂双环[3.3.1]壬烷-3-醇的合成工艺优化  

Optimization of Synthesis Technology of 9-Benzyl-9-azabicyclo[3.3.1]nonan-3-ol

作　　者：白雪燕 李晓阳 葛健 朱诚 吴志平 BAI Xueyan;LI Xiaoyang;GE Jian;ZHU Cheng;WU Zhiping(Laboratory of Antitumor Pharmacology,College of Life Science,China Jiliang University, Department of Food Science,China Jiliang University,Hangzhou,Zhejiang 310018,China)

机构地区：[1]中国计量大学生命科学学院抗肿瘤药物药理学实验室食品科学系,浙江杭州310018

出　　处：《化学世界》2018年第12期815-820,共6页Chemical World

基　　金：浙江省科技发展计划(No.2016C33081)资助项目

摘　　要：利用Mannich反应合成9-苄基-9-氮杂双环[3.3.1]壬烷-3-酮。选择异丙醇铝为催化剂还原9-苄基-9-氮杂双环[3.3.1]壬烷-3-酮。在单因素试验基础上,采用正交试验考察9-苄基-9-氮杂双环[3.3.1]壬烷-3-酮与异丙醇铝物质的量之比、异丙醇的用量、原料滴加速度和反应时间,四个因素对产率的影响。最佳的合成条件为:n(9-苄基-9-氮杂双环[3.3.1]壬烷-3-酮)∶n(异丙醇铝)=1∶0.5,异丙醇30mL,滴加速度为3s滴1滴,反应时间6h,产率为89.6%～90.8%。9-Benzyl-9-azabicyclo[3.3.1]nonane-3-ol was synthesized from the reduction of 9-benzyl-9-azabicyclo[3.3.1]nonane-3-one via Mannich reaction by using aluminum isopropoxide as reductant.Based on the single-factor experiment,orthogonal tests were conducted to study the effects of material ratio,amounts of isopropanol,dropping speed of the reductant solution and reaction time on the yield.When the amounts of n(9-benzyl-9-azabicyclo[3.3.1]nonane-3-one)∶n(aluminium isopropoxide)=1∶0.5,and isopropanol are 30 mL,the reaction yield can reach up to 89.6%~90.8% with a 1 drops in 3 sspeed of the reductant solution and a 6 hreaction time.

关 键 词：MANNICH反应 9-苄基-9-氮杂双环[3.3.1]壬烷-3-醇 正交试验 还原反应 

分 类 号：O641.4[理学—物理化学]