WestCHEM, School of Chemistry, University of Glasgow, University Avenue, Glasgow G12 8QQ, UK.
Nat Chem. 2012 Dec;4(12):1037-43. doi: 10.1038/nchem.1489. Epub 2012 Nov 18.
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.
多相合成可以既耗时又受到缺乏重现性的限制。目前在有机合成中很常见的流动系统方法尚未广泛用于簇合物的合成。在此，我们将自动化的流动过程与多次分批结晶相结合，用于筛选和扩大多金属氧酸盐和锰基单分子磁体的合成。通过编程多泵反应器系统来顺序改变反应条件，从而在比传统方法更短的时间内探索更大的参数空间，实现了这些结构的放大合成。此外，还展示了该阵列作为发现工具的潜力。可以从反应阵列中轻松识别出用于产物分离的成功条件，然后通过简单地连续应用这些流动条件，就可以立即获得“放大”的直接途径。在所有情况下，都获得了大量的纯相材料，并且发现、重复和放大的时间都减少了。
