Department of Applied Chemistry, School of Engineering, The University of Tokyo , 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656, Japan.
J Am Chem Soc. 2014 Dec 31;136(52):17899-901. doi: 10.1021/ja5109535. Epub 2014 Dec 15.
We have developed a new synthetic protocol for the preparation of a microcrystalline powder (median size: X50 = 25 μm) of networked M6L4 cages 1a for the stationary phase of an affinity column on a greater than 50 g scale. Analogously to large single crystals 1b (X50 ≈ 0.5 mm), microcrystals 1a accommodate guest molecules tetrathiafulvalene (TTF) and fullerene (C60) at up to 32 and 35 wt %, respectively. Importantly, the host-guest interactions within networked cages could be evaluated in terms of the retention time from HPLC analysis by using microcrystals 1a as the stationary phase. In this way, favorable guests for networked cages 1 and even solution M6L4 cage 2 could easily be assessed by HPLC.
我们开发了一种新的合成方案，用于制备网络状 M6L4 笼 1a 的微晶粉末（中值粒径：X50 = 25 μm），用于在大于 50 g 规模上制备亲和柱的固定相。类似于大单晶 1b（X50 ≈ 0.5 毫米），微晶 1a 可以容纳客体分子四硫富瓦烯（TTF）和富勒烯（C60），分别高达 32wt%和 35wt%。重要的是，通过使用微晶 1a 作为固定相进行 HPLC 分析，可以根据保留时间来评估网络状笼内的主客体相互作用。通过这种方式，很容易通过 HPLC 评估对网络状笼 1 有利的客体，甚至溶液状 M6L4 笼 2。
