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Method for separating phenylsuccinic acid enantiomer by extraction from multi-stage centrifugal inclusion reaction

A technology for phenylsuccinic acid and enantiomers is applied in the field of extraction and separation of enantiomers of phenylsuccinic acid by countercurrent inclusion reaction of a multistage centrifugal extractor, and can solve the problems of excess enantiomer and low yield, etc. To achieve the effect of stable product quality, easy operation and improved purity

Inactive Publication Date: 2012-10-03
唐课文 +2
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Problems solved by technology

[0005] This patent proposes a method for separating phenylsuccinic acid enantiomers by single-stage chiral solvent extraction to separate enantiomers of phenylsuccinic acid with enantiomer excess and low yield—using multistage centrifugal extraction Method for extracting and separating enantiomers of phenylsuccinic acid by countercurrent inclusion reaction

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  • Method for separating phenylsuccinic acid enantiomer by extraction from multi-stage centrifugal inclusion reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0012] 0.7687g of phenylsuccinic acid enantiomer was dissolved in n-octanol organic solvent to form a 4L solution with a concentration of 1mM as the material liquid phase, and pure n-octanol organic solvent was used as the organic phase.

[0013] Take 57.6400g water-soluble hydroxypropyl-β-cyclodextrin and dissolve it in 0.1M NaH 2 PO 4 / H 3 PO 4 Adjust the pH of the buffer solution to 3.0 to prepare 4L of aqueous solution with a concentration of 0.01M as the extraction phase.

[0014] 8-stage centrifuges in series, using a centrifugal pump to pump the organic phase into the centrifuge first, when the organic phase flows out of the outlet, pump the aqueous phase extraction phase into the centrifuge from the corresponding inlet, after a period of time reaches equilibrium and then the liquid The phase is pumped in from the 4th stage centrifuge. The volume ratio of aqueous phase extraction phase: organic phase is 0.8:1, and the volume ratio of aqueous phase extraction phase: ...

Embodiment 2

[0016] 0.7687g phenylsuccinic acid enantiomer was dissolved in 1.2-dichloroethane organic solvent to prepare 4L solution with a concentration of 1mM as the material liquid phase, and pure 1.2-dichloroethane organic solvent as the organic phase.

[0017] Take 57.6400g water-soluble hydroxypropyl-β-cyclodextrin and dissolve it in 0.1M NaH 2 PO 4 / H 3 PO 4 Adjust the pH of the buffer solution to 3.0 to prepare 4L of aqueous solution with a concentration of 0.01M as the extraction phase.

[0018] 8-stage centrifuges in series, using a centrifugal pump to pump the organic phase into the centrifuge first, when the organic phase flows out of the outlet, pump the aqueous phase extraction phase into the centrifuge from the corresponding inlet, after a period of time reaches equilibrium and then the liquid The phase is pumped in from the 4th stage centrifuge. The volume ratio of aqueous extraction phase: organic phase is 1.5:1, and the volume ratio of aqueous extraction phase: solid...

Embodiment 3

[0020] Take 1.5374g of phenylsuccinic acid enantiomers and dissolve them in n-octanol organic solvent to form a 4L solution with a concentration of 2mM as the material liquid phase, and use pure n-octanol organic solvent as the organic phase.

[0021] Take 115.2800g water-soluble hydroxypropyl-β-cyclodextrin and dissolve it in 0.1M NaH 2 PO 4 / H 3 PO 4 Adjust the pH of the buffer solution to 2.5 to prepare 4L aqueous solution with a concentration of 0.02M as the extraction phase.

[0022] Connect 20-stage centrifuges in series, use a centrifugal pump to pump the organic phase into the centrifuge first, when the organic phase flows out from the outlet end, pump the aqueous phase extraction phase into the centrifuge from the corresponding inlet, after a period of time reaches equilibrium and then the liquid The phase is pumped in from the 10th stage centrifuge. The volume ratio of aqueous extraction phase: organic phase is 0.5:1, and the volume ratio of aqueous extraction ph...

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Abstract

The invention discloses a method for separating phenylsuccinic acid enantiomer by extraction, specifically a method for separating phenylsuccinic acid enantiomer by extraction from reflux inclusion reaction in a multi-stage centrifugal extractor. Through selective inclusion of water-soluble beta-cyclodextrin and the phenylsuccinic acid enantiomer and centrifugal force of the centrifugal extractor, the water phase and the organic phase have strengthened mass transfer efficiency under the action of centrifugal force so as to speed up the inclusion reaction and mass transfer efficiency of the phenylsuccinic acid enantiomer in the water phase and the organic phase. By the technology, the problems of low mass transfer efficiency and low purification of single-stage extraction in the common extraction technology are solved. According to this method, fast and high-selectivity separation of phenylsuccinic acid can be implemented by multi-stage balance extraction. Moreover, the device is simple and the operation is easy and simple to handle.

Description

technical field [0001] The invention relates to a method for extracting and separating the enantiomers of phenylsuccinic acid, in particular to a method for extracting and separating the enantiomers of phenylsuccinic acid by countercurrent inclusion reaction of a multistage centrifugal extractor. Background technique [0002] Phenylsuccinic acid (PSA), that is, phenylsuccinic acid, is an important intermediate of N-methyl-α-phenylsuccinimide (phensuxi mide), and (S )- ( + ) - PSA is a good chiral resolving agent for chlorpheniramine, and can be used as a chiral selector for synthesis of liquid chromatography chiral fixation. Therefore, it is necessary to study the chiral resolution of PSA enantiomers. [0003] At present, the methods for obtaining single chiral drug enantiomers at home and abroad can be mainly divided into three categories: extraction of chiral drugs from natural products, asymmetric synthesis and racemate resolution. The racemate resolution method has att...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/10C07C51/48
CPCY02P20/582
Inventor 唐课文刘永兵张盼良张辉周从山易健民杨长安
Owner 唐课文
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