Family of Conglomerate-Forming Systems Composed of Chlocyphos and Alkyl-amine. Assessment of Their Resolution Performances by Using Various Modes of Preferential Crystallization

The present study aimed at screening conglomerate derivatives of racemic chlocyphos (4-(2-chlorophenyl)-5,5-dimethyl-2-hydroxy-1,3,2-dioxaphosphorinane 2-oxide) and to perform enantiomeric separation by preferential crystallization. A list of more than 20 chlocyphos salt derivatives were characteriz...

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Bibliographic Details
Published in:Crystal growth & design 2019-09, Vol.19 (9), p.5173-5183
Main Authors: Mbodji, Aliou, Gbabode, Gabin, Sanselme, Morgane, Couvrat, Nicolas, Leeman, Michel, Dupray, Valérie, Kellogg, Richard M, Coquerel, Gérard
Format: Article
Language:English
Subjects:
Chemical Sciences
Cristallography
Engineering Sciences
Inorganic chemistry
Materials
Organic chemistry
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Summary:The present study aimed at screening conglomerate derivatives of racemic chlocyphos (4-(2-chlorophenyl)-5,5-dimethyl-2-hydroxy-1,3,2-dioxaphosphorinane 2-oxide) and to perform enantiomeric separation by preferential crystallization. A list of more than 20 chlocyphos salt derivatives were characterized by various techniques (SHG, DSC, and X-ray powder diffraction). A family of salts formed with various alkyl amines crystallizing as conglomerates is evidenced. The first attempts to resolve these conglomerates by preferential crystallization at small scale were successful. The mitigated performances of these entrainments are discussed.
ISSN:1528-7483
1528-7505
DOI:10.1021/acs.cgd.9b00568