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Method for separating naproxen enantiomers by adopting centrifugal extractor and carrying out multi-stage counter current extraction

A naproxen and enantiomer technology is applied in the field of using a centrifugal extractor to extract and separate naproxen enantiomers through multi-stage countercurrent reaction extraction, which can solve the problems of low separation purity and yield, and achieve stable product quality and process flow. Simplicity, the effect of improving purity and yield

Inactive Publication Date: 2015-04-29
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] This patent proposes a new method for separating naproxen enantiomers in view of the difficult problems of separation purity and low yield of naproxen enantiomers—the method of separating naproxen enantiomers by multi-stage countercurrent extraction with a centrifugal extractor. method

Method used

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  • Method for separating naproxen enantiomers by adopting centrifugal extractor and carrying out multi-stage counter current extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Get 0.5757 g naproxen enantiomer dissolved in 1,2-dichloroethane to make a concentration of 1 L solution of 2.5 mmol / L as material liquid phase;

[0014] Take 147.1 g HP-β-CD and dissolve it in 0.1 mol / L NaH 2 PO 4 / H 3 PO 4 Adjust the pH in the buffer solution to 2.5 to form a 2 L solution with a concentration of 0.05 mol / L as the aqueous phase;

[0015] Take pure 1,2-dichloroethane solvent as the organic phase;

[0016] 10-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 6th stage centrifuge. Organic phase: solid-liquid phase volume ratio 2:1, water phase: organic phase volume ratio 7.4:1. Perform 10-stage centrifugal countercurrent extraction at room temperature for 3-4 hours...

Embodiment 2

[0018] Get 0.5757 g naproxen enantiomer dissolved in 1,2-dichloroethane to make a concentration of 1 L solution of 2.5 mmol / L as material liquid phase;

[0019] Take 147.1 g HP-β-CD and dissolve it in 0.1 mol / L NaH 2 PO 4 / H 3 PO 4 Adjust the pH in the buffer solution to 2.5 to form a 2 L solution with a concentration of 0.05 mol / L as the aqueous phase;

[0020] Take pure 1,2-dichloroethane solvent as the organic phase;

[0021] 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 11th stage centrifuge. Organic phase: solid-liquid phase volume ratio 2:1, water phase: organic phase volume ratio 7.4:1. Perform 10-stage centrifugal countercurrent extraction at room temperature ...

Embodiment 3

[0023] Get 1.1514 g of naproxen enantiomers dissolved in 1,2-dichloroethane to make a concentration of 1 L solution of 5.0 mmol / L as the material liquid phase;

[0024] Take 294.2 g HP-β-CD and dissolve in 0.1 mol / L NaH 2 PO 4 / H 3 PO 4 Adjust the pH in the buffer solution to 2.5 to form a 2 L solution with a concentration of 0.1 mol / L as the aqueous phase;

[0025] Take pure 1,2-dichloroethane solvent as the organic phase;

[0026] 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 11th stage centrifuge. Organic phase: solid-liquid phase volume ratio 2:1, water phase: organic phase volume ratio 4.4:1. Perform 20-stage centrifugal countercurrent extraction at room temperat...

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Abstract

The invention relates to a method for separating naproxen enantiomers by adopting a centrifugal extractor and carrying out multi-stage counter current extraction. The invention provides a new method for separating the naproxen enantiomers. The method for separating the naproxen enantiomers is characterized in that the naproxen enantiomers are selectively distributed in an organic phase / aqueous phase in a three-dimensional way due to selective complexation between water-soluble beta-cyclodextrin and the naproxen enantiomers; and the aqueous phase and the organic phase are rapidly mixed and rapidly separated by virtue of a centrifugal acting force of the centrifugal extractor, so that transmission and reaction of the naproxen enantiomers in the aqueous phase and the organic phase are accelerated. The method for separating the naproxen enantiomers has the advantages that the problems that mass transfer efficiency of a general extraction technique is low and product purity is low are overcome; rapid and high-selectivity separation on the naproxen enantiomers is realized by carrying out multi-stage equilibrium extraction; meanwhile, equipment adopted by the method provided by the invention is simple and is easy to operate.

Description

technical field [0001] The invention relates to a method for extracting and separating naproxen enantiomers, in particular to a method for extracting and separating naproxen enantiomers through a multistage countercurrent reaction using a centrifugal extractor. Background technique [0002] Naproxen, α-methyl-6-methoxy-2-naphthaleneacetic acid, is an important non-steroidal anti-inflammatory, antipyretic and analgesic drug, mainly used in the treatment of rheumatoid arthritis, rheumatic spondylosis Inflammation and postpartum, postoperative pain relief and other diseases. There is a chiral carbon atom in its α-position, and there is a pair of optical isomers. The anti-inflammatory activity of S-naproxen in the body is 28 times that of R-type. In order to reduce the dosage and the toxicity to the human body side effects, it must be chiral resolved. Therefore, it is of great significance to develop a preparation method for the single enantiomer of naproxen. [0003] The pre...

Claims

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Application Information

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IPC IPC(8): C07C59/64C07C51/48
CPCC07C51/48
Inventor 唐课文张盼良文平周从山杨长安易健民阎建辉
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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