A flow-system array for the discovery and scale up of inorganic clusters

A flow-system array for the discovery and scale up of inorganic clusters
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DOI:
10.1038/nchem.1489
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发表时间:
2012-12-01
期刊:
影响因子:
21.8
通讯作者:
Cronin, Leroy
Cronin, Leroy
中科院分区:
化学1区
文献类型:
--
作者:
Richmond, Craig J.;Miras, Haralampos N.;Cronin, Leroy

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无机簇合物的批量合成可能既耗时又受到缺乏再现性的限制。流动体系方法,现在常见的有机合成,还没有被广泛使用的簇的合成。在这里,我们联合收割机了自动化流程与多批次结晶的筛选和规模的合成聚氧乙烯酸盐和锰基单分子磁体。通过编程多泵反应器系统来顺序地改变反应条件,从而在比常规可能的时间更短的时间内探索更大的参数空间,实现了这些架构的合成的放大。此外,使用阵列作为发现工具的潜力被证明。从一系列反应中很容易确定成功的产物分离条件,然后通过连续应用这些流动条件即可立即获得“放大”的直接途径。在所有情况下,获得了大量的纯相材料,并且发现、重复和放大所需的时间减少了。
The batch synthesis of inorganic clusters can be both time consuming and limited by a lack of reproducibility. Flow-system approaches, now common in organic synthesis, have not been utilized widely for the synthesis of clusters. Herein we combine an automated flow process with multiple batch crystallizations for the screening and scale up of syntheses of polyoxometalates and manganese-based single-molecule magnets. Scale up of the synthesis of these architectures was achieved by programming a multiple-pump reactor system to vary reaction conditions sequentially, and thus explore a larger parameter space in a shorter time than conventionally possible. Also, the potential for using the array as a discovery tool is demonstrated. Successful conditions for product isolation were identified easily from the array of reactions, and a direct route to 'scale up' was then immediately available simply by continuous application of these flow conditions. In all cases, large quantities of phase-pure material were obtained and the time taken for the discovery, repetition and scale up decreased.