Continuous Consecutive Reactions with Inter-Reaction Solvent Exchange by Membrane Separation.
Continuous Consecutive Reactions with Inter-Reaction Solvent Exchange by Membrane Separation.
复制标题
DOI：
10.1002/anie.201607795
复制
发表时间：
2016-10-17
影响因子：
16.6
通讯作者：
Livingston, Andrew
中科院分区：
文献类型：
--
作者：
Peeva, Ludmila;Burgal, Joao Da Silva;Heckenast, Zsofia;Brazy, Florine;Cazenave, Florian;Livingston, Andrew
药物生产通常涉及多个反应步骤，在连续反应之间存在分离。在多步合成中使从间歇操作到连续操作的过渡复杂化的两个过程是溶剂交换（特别是高沸点溶剂到低沸点溶剂）和催化剂分离。这里展示的是膜分离作为在连续操作期间进行这些过程的使能平台。两个连续的反应在不同的溶剂中进行，通过连续流动膜单元实现催化剂分离和反应间溶剂交换。在保留催化剂的连续膜反应器中，在N，N-二甲基甲酰胺（DMF）中进行Heck偶联反应。Heck反应产物在逆流膜系统中进行溶剂交换，其中DMF被乙醇连续取代。在交换之后，溶解在乙醇中的产物通过填充有铁催化剂的柱，并且经历还原（> 99%产率）。
Pharmaceutical production typically involves multiple reaction steps with separations between successive reactions. Two processes which complicate the transition from batch to continuous operation in multistep synthesis are solvent exchange (especially high‐boiling‐ to low‐boiling‐point solvent), and catalyst separation. Demonstrated here is membrane separation as an enabling platform for undertaking these processes during continuous operation. Two consecutive reactions are performed in different solvents, with catalyst separation and inter‐reaction solvent exchange achieved by continuous flow membrane units. A Heck coupling reaction is performed in N,N‐dimethylformamide (DMF) in a continuous membrane reactor which retains the catalyst. The Heck reaction product undergoes solvent exchange in a counter‐current membrane system where DMF is continuously replaced by ethanol. After exchange the product dissolved in ethanol passes through a column packed with an iron catalyst, and undergoes reduction (>99 % yield).
登录
查看更多内容
影响因子：
5.4
作者：
Liu, YG;Lu, YS;Blacklock, TJ
通讯作者：
Blacklock, TJ
影响因子：
9.5
作者：
Sheth, JP;Qin, YJ;Baltzis, BC
通讯作者：
Baltzis, BC
影响因子：
7.3
作者：
Peeva, Ludmila;Burgal, Joao da Silva;Livingston, Andrew G.
通讯作者：
Livingston, Andrew G.
影响因子：
3.6
作者：
Caron, S;Vazquez, E;Murata, Y
通讯作者：
Murata, Y
DOI：
10.1111/j.1749-6632.2003.tb05996.x
发表时间：
2003-01-01
期刊：
ADVANCED MEMBRANE TECHNOLOGY
影响因子：
--
作者：
Livingston, A;Peeva, L;Dos Santos, LMF
通讯作者：
Dos Santos, LMF