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Method for separating and purifying Clofarabine

A technology for separation and purification of clofarabine, applied in the field of separation and purification of crude clofarabine, can solve the problems of large amount of solvent, large pollution, low purity of clofarabine and the like

Active Publication Date: 2012-08-01
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Methanol is more toxic, and the amount of solvent used is large, and the pollution is large, and the purity of the final obtained clofarabine is low

Method used

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  • Method for separating and purifying Clofarabine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Dissolving and filtering:

[0027] Get clofarabine crude product 3.75g, be dissolved in 750mL of boiling aqueous solution, solid clofarabine crude product is dissolved, after dissolving, filter with the organic microporous membrane of 0.45 μm, obtain the solution of 5mg / mL, prepare clofarabine as the next step raw material.

[0028] (2) separation and purification:

[0029] Inject 18 mL of the solution diluted in step (1) into a reversed-phase high-efficiency preparative liquid chromatograph, the mobile phase is composed of acetonitrile-water, the volume ratio of acetonitrile-water is 1:8.8, isocratic elution, flow rate 80mL / min , UV detector online detection, detection wavelength 254nm. The preparation components of clofarabine are collected in a targeted manner to obtain a clofarabine solution.

[0030] (3) Product recycling

[0031] Acetonitrile and water in the clofarabine solution obtained by step (2) high-efficiency preparative liquid chromatography separa...

Embodiment 2

[0033] (1) Dissolving and filtering:

[0034] Take 3.75g of crude clofarabine, dissolve it in 577mL of boiling aqueous solution, dissolve the crude solid clofarabine, and filter it with a 0.45μm organic microporous membrane to obtain a 6.5mg / mL solution, which is used as the next step to prepare clofarabine raw materials.

[0035] (2) separation and purification:

[0036] Inject 15 mL of the solution diluted in step (1) into a reversed-phase high-efficiency preparative liquid chromatograph, the mobile phase is composed of acetonitrile-water, the volume ratio of acetonitrile-water is 1:9, isocratic elution, flow rate 85mL / min , UV detector online detection, detection wavelength 254nm. The preparation components of clofarabine are collected in a targeted manner to obtain a clofarabine solution.

[0037] (3) Product recycling

[0038] Acetonitrile and water in the clofarabine solution obtained by step (2) high-efficiency preparative liquid chromatography separation are remove...

Embodiment 3

[0040] (1) Dissolving and filtering

[0041] Take 3.75g of the crude product of clofarabine, dissolve it in 469mL of boiling aqueous solution, dissolve the crude product of solid clofarabine, and filter it with an organic microporous membrane of 0.45 μm after dissolving to obtain a solution of 8 mg / mL, which is used as the next step to prepare clofarabine raw material.

[0042] (2) Separation and purification

[0043] Inject 18 mL of the solution diluted in step (1) into a reversed-phase high-efficiency preparative liquid chromatograph, the mobile phase is composed of acetonitrile-water, the volume ratio of acetonitrile-water is 1:9.2, isocratic elution, flow rate 90mL / min , UV detector online detection, detection wavelength 254nm. The preparation components of clofarabine are collected in a targeted manner to obtain a clofarabine solution.

[0044] (3) Product recycling

[0045] Acetonitrile and water in the clofarabine solution obtained by step (2) separated by high-effi...

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Abstract

The invention belongs to pharmaceutical technical field, and provides a method for separating and purifying Clofarabine, the method comprises the following steps: a step of dissolving and filtering, a step of separating and purifying by high performance preparative liquid chromatography, a step of recovering products and the like, wherein the step of separating and purifying employs inverse high performance preparative liquid chromatography, the mobile phase is an acetonitrile solution, and an UV detector carries out on-line detection. The method of the invention has the advantages of simple operation, high separation efficiency, stable technology and low cost, and separation with high purify of mass Clofarabine can be realized, the purity is more than 99.8% and the yield is more than 98%.

Description

technical field [0001] The invention relates to the field of pharmaceutical synthesis, in particular to a method for separating and purifying crude clofarabine. Background technique [0002] Clofarabine, chemical name: 2-chloro-9-(2-deoxy-2-fluoro-β-D-arabinofuran)-9H-purin-6-amine, 2-chloro-9-(2 -deoxy-2-fluoro-β-D-arabinofuranosyl)-9H-purin-6-amine; CAS number: 123318-82-1; Molecular formula: C 10 h 11 ClFN 5 o 3 ; Molecular weight 303.68; Its structural formula is: [0003] [0004] Clofarabine is a second-generation purine nucleoside derivative developed by the Southern Research Institute (CRO) in the United States. It was approved by the FDA in December 2004 and EMEA in Europe in May 2006 for pediatric patients. Relapsed or refractory ALL after at least 2 previous treatment regimens, and are listed as orphan drug products by the US FDA and the EU, respectively. Clofarabine is the first new drug approved specifically for the treatment of childhood acute leukemia...

Claims

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Application Information

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IPC IPC(8): C07H19/173C07H1/06
Inventor 赵志全王洪锋张召军
Owner SHANDONG NEWTIME PHARMA
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