Thakur Nimisha, Patil Rahul A, Talebi Mohsen, Readel Elizabeth R, Armstrong Daniel W
Department of Chemistry and Biochemistry, University of Texas at Arlington, Arlington, Texas.
Chirality. 2019 Sep;31(9):688-699. doi: 10.1002/chir.23086. Epub 2019 Jul 18.
The enantiomeric excess of chiral starting materials is one of the important factors determining the enantiopurity of products in asymmetric synthesis. Fifty-one commercially available chiral reagents used as building blocks, catalysts, and auxiliaries in various enantioselective syntheses were assayed for their enantiomeric purity. The test results were classified within five impurities level (ie, <0.01%, 0.01%-0.1%, 0.1%-1%, 1%-10%, >10%). Previously from 1998 to 2013, several reports have been published on the enantiomeric composition of more than 300 chiral reagents. This series of papers is necessitated by the fact that new reagents are forthcoming and that the enantiomeric purity of the same reagent can vary from batch to batch and/or from supplier to supplier. This report presents chiral liquid chromatography (LC) and gas chromatography (GC) methods to separate enantiomers of chiral compounds and evaluate their enantiomeric purities. The accurate and efficient LC analysis was done using newly introduced superficially porous particle (SPP 2.7 μm) based chiral stationary phases (TeicoShell, VancoShell, LarihcShell-P, and NicoShell).
手性起始原料的对映体过量是决定不对称合成中产物对映体纯度的重要因素之一。对51种在各种对映选择性合成中用作结构单元、催化剂和助剂的市售手性试剂进行了对映体纯度测定。测试结果分为五个杂质水平（即<0.01%、0.01%-0.1%、0.1%-1%、1%-10%、>10%）。此前在1998年至2013年期间，已发表了多篇关于300多种手性试剂对映体组成的报告。由于新试剂不断涌现，且同一试剂的对映体纯度可能因批次不同和/或供应商不同而有所差异，因此有必要撰写这一系列论文。本报告介绍了用于分离手性化合物对映体并评估其对映体纯度的手性液相色谱（LC）和气相色谱（GC）方法。使用新引入的基于表面多孔颗粒（2.7μm SPP）的手性固定相（TeicoShell、VancoShell、LarihcShell-P和NicoShell）进行了准确高效的LC分析。
