Origins of Batch-to-Batch Variation: Organoindium Reagents from Indium Metal.
Origins of Batch-to-Batch Variation: Organoindium Reagents from Indium Metal.
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DOI：
10.1021/acs.organomet.0c00417
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发表时间：
2020-07-27
期刊：
影响因子：
2.8
通讯作者：
Blum SA
中科院分区：
文献类型：
--
作者：
Jess K;Hanada EM;Peacock H;Blum SA
先前报道了由铟金属合成的有机铟试剂的产率高度依赖于金属批次和供应商，这是由于抗结块剂的存在或不存在。在这里，单颗粒荧光显微镜确定，MgO，在一些批次中名义上用于防结块的添加剂，显着增加了小分子有机物的物理吸附到所得MgO涂覆的铟金属颗粒的表面上。一种惰性的和相对非极性的硼dipyrromethene荧光团与烃尾巴提供了一个敏感的探针，这种表面物理吸附。SEM图像显示，铟颗粒的表面性质显着不同，无论是有或没有MgO，与荧光显微镜观察到的不同的物理吸附性能相一致。我们进一步记录了我们实验室和之前文献中关于该防结块剂的存在和组成的不完整商业瓶标签，这可能使实验室之间的重现性复杂化。三甲基甲硅烷基氯化物预处理，一个步骤中采用的一个子集的合成程序，去除了防结块剂和生产的颗粒具有类似的物理吸附性能的商业批次的铟粉分布没有防结块剂。这些数据表明，一个额外的基板/催化剂物理吸附机制的可能性，通过该防结块剂可能会影响合成过程中产生的有机铟试剂从铟金属，除了简单的防结块。
Yields of organoindium reagents synthesized from indium metal were previously reported to be highly dependent on metal batch and supplier due to the presence or absence of anticaking agent. Here, single-particle fluorescence microscopy established that MgO, an additive in some batches nominally for anticaking, significantly increased the physisorption of small-molecule organics onto the surface of the resulting MgO-coated indium metal particles. An inert and relatively nonpolar boron dipyrromethene fluorophore with a hydrocarbon tail provided a sensitive probe for this surface physisorption. SEM images revealed markedly different surface properties of indium particles either with or without MgO, consistent with their different physisorption properties observed by fluorescence microscopy. We further documented incomplete commercial bottle labeling regarding the presence and composition of this anticaking agent, both within our laboratory and previously in the literature, which may complicate reproducibility between laboratories. Trimethylsilyl chloride pretreatment, a step employed in a subset of reported synthetic procedures, removed the anticaking agent and produced particles with similar physisorption properties as commercial batches of indium powder distributed without the anticaking agent. These data indicate the possibility of an additional substrate/catalyst physisorption mechanism by which the anticaking agent may be influencing synthetic procedures that generate organoindium reagents from indium metal, in addition to simple anticaking.
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影响因子：
3.6
作者：
Arvela, RK;Leadbeater, NE;Singer, RD
通讯作者：
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影响因子：
64.8
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Silberberg, Shai D.
影响因子：
3.6
作者：
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Minehan, Thomas
影响因子：
3.6
作者：
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通讯作者：
Yoshikai, Naohiko
影响因子：
2.1
作者：
Adak, Laksmikanta;Yoshikai, Naohiko
通讯作者：
Yoshikai, Naohiko