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

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.