scholarly journals Efficient resolution of racemic crown-shaped cyclotriveratrylene derivatives and isolation and characterization of the intermediate saddle isomer

2019 ◽  
Vol 15 ◽  
pp. 1339-1346
Author(s):  
Sven Götz ◽  
Andreas Schneider ◽  
Arne Lützen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Nmr Spectroscopy ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Hplc Separation ◽  
Promising Alternative ◽  
Isolation And Characterization ◽  
C Nmr

The preparative resolution of a trifunctionalized C 3-symmetrical chiral cyclotriveratrylene derivative was achieved via high-performance liquid chromatography (HPLC) on a chiral stationary phase. This approach is a promising alternative to the previously reported resolution through formation of diastereomeric esters because it involves fewer synthetic steps and is less prone to thermal (re)racemization. During these studies an intermediate saddle conformer could also be isolated and characterized by 1H and 13C NMR spectroscopy. The HPLC separation method was further developed in order to allow investigations on the racemization behavior of the cyclotriveratrylene derivative.

scholarly journals Synthesis, Isolation and Characterization of Process-Related Impurities in Oseltamivir Phosphate

2012 ◽  
Vol 9 (1) ◽  
pp. 113-120 ◽  
Author(s):  
Yogesh Kumar Sharma ◽  
Dau Dayal Agarwal ◽  
Sudesh Bhure ◽  
Sanjay Singh Rathore ◽  
Chakravir Rawat ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Mass Number ◽  
Reverse Phase ◽  
Related Impurities ◽  
Isolation And Characterization ◽  
Bulk Drug ◽  
Oseltamivir Phosphate

Three known impurities in oseltamivir phosphate bulk drug at level 0.1% (ranging from 0.05-0.1%) were detected by gradient reverse phase high performance liquid chromatography. These impurities were preliminarily identified by the mass number of the impurities. Different experiments were conducted and finally the known impurities were synthesized and characterized.

scholarly journals Homochiral Metal–Organic Framework [Co(L)(bpe)2(H2O)2]·H2O Used for Separation of Racemates in High-Performance Liquid Chromatography

2021 ◽  
Author(s):  
Yunyan Yu ◽  
Baoyan Yuan ◽  
Cong Hu ◽  
Nan Fu ◽  
Nayan Xu ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Metal Organic Framework ◽  
Hplc Separation ◽  
Relative Standard ◽  
Metal Organic ◽  
Cyclohexanedicarboxylic Acid ◽  
Organic Framework

Abstract A homochiral metal–organic framework (MOF) comprising [Co(L)(bpe)2(H2O)2]·H2O was prepared using (1R,2R)-(−)-1,2-cyclohexanedicarboxylic acid (H2L) and 1,2-bis(4-pyridyl)-ethylene as organic ligands. The homochiral MOF [Co(L)(bpe)2(H2O)2]·H2O was explored as chiral stationary phase (CSP) for high-performance liquid chromatography (HPLC) separation of racemates. Nine racemates including naphthol, alcohol, diol, amine, ketone, ether and organic acid were well separated on the homochiral MOF [Co(L)(bpe)2(H2O)2]·H2O column (250 mm long × 4.6 mm i.d.). The relative standard deviation for five replicate separations of 1,1′-bi-2-naphthol is 0.69% for the retention time, indicating that the good reproducibility and stability of the homochiral MOF column for HPLC enantioseparation. The results indicated that the homochiral MOF as CSP is practical, which promotes the application of homochiral MOFs in HPLC.

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