High-performance liquid chromatographic separation of enantiomers and diastereomers of 2-methylcyclohexanone thiosemicarbazone, and determination of absolute configuration and configurational stability.
J Chromatogr A
; 1172(2): 160-9, 2007 Nov 23.
Article
em En
| MEDLINE
| ID: mdl-17959189
ABSTRACT
Simultaneous HPLC diastereo- and enantioseparations of 2-methylcyclohexanone thiosemicarbazone (2-MCET) were accomplished on coated- and immobilized type polysaccharide-based chiral stationary phases (CSPs). The identification of all stereoisomeric forms and their stereochemistry were achieved by combining theoretical, HPLC and chiroptical data. The stereochemical stability of the target compound was studied by classical off-column and dynamic HPLC kinetic procedures and the influence of different parameters such solvent, TFA concentration and temperature on stereoisomerization process was evaluated. The findings obtained by chromatographic and kinetic experiments were used to develop a simple method to convert the racemic form of 2-MCET into a single enantiomer.
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Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Tiossemicarbazonas
/
Cromatografia Líquida de Alta Pressão
/
Dicroísmo Circular
/
Cicloexanonas
Tipo de estudo:
Prognostic_studies
Idioma:
En
Revista:
J Chromatogr A
Ano de publicação:
2007
Tipo de documento:
Article
País de afiliação:
Itália