Novel cyclic extraction and diastereomer crystallization coupling method for efficient chiral resolution and mother liquor in-situ regeneration

Abstract

The invention discloses a novel cyclic extraction and diastereomer crystallization coupling method for efficient chiral resolution and mother liquor in-situ regeneration. The method comprises the steps of respectively selectively crystallizing and separating out a levorotatory body and a dextrorotatory body through a levorotatory crystallizer and a dextrorotatory crystallizer; and carrying out circulating liquid-liquid extraction by adding an extraction phase and mother liquor of the two crystallizers, so that mutual transfer of respective uncrystallized enantiomers between the two mother liquor is realized. An uncrystallized dextrorotatory body in the levorotatory crystallizer istransferred to the dextrorotatory crystallizer, and an uncrystallized levorotatory body in the dextrorotatory crystallizer is istransferred to the levorotatory crystallizer. Compared with a traditional diastereomer crystallization method, the method has the advantages that the resolution effect is better (thepurity and the yield are improved), and in-situ regeneration (transfer of uncrystallized enantiomers) and repeated application of the mother liquor are realized. Repeated crystallization is carried out by supplementing raceme and a resolving agent into the mother liquor, so that two high-purity enantiomers can be continuously produced. According to the invention, the problems of low total yield and mother liquor treatment of the traditional diastereomer crystallization method are solved.

Description

technical field [0001] The invention relates to a method for high-efficiency chiral separation and in-situ regeneration of mother liquor, belonging to the technical field of chemical separation engineering. Especially suitable for chiral resolution of chiral drugs, pesticides and their intermediates. Background technique [0002] The amino acids and sugars that make up human tissues are single enantiomers, which makes the human body have a highly asymmetric chiral environment. This leads to significant differences in the pharmacological effects of the two enantiomers of chiral drugs (for example, one enantiomer has curative effect on the human body, while the other has no curative effect or even has toxic side effects). Due to the ubiquity of chiral carbon atoms, many organic drug molecules are chiral. The general physical and chemical properties of the left-handed and right-handed enantiomers of chiral drugs are the same, and there are only differences in properties such ...

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Problems solved by technology

[0006] Aiming at the technical problems existing in the traditional diastereomeric crystallization resolution method, such as "difficult to balance the purity and yield of crystal products" and "treatment and repeated application of crystallization mother liquor", the present invention provides a high-efficiency chiral resolution and A New Separation Method Coupled with Circular Extraction and Diastereomeric Crystallization for In Situ Regeneration of Mother Liquor

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