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Method for purifying pomalidomide

A purification method, the technology of polilidomide, which is applied in the direction of organic chemistry, can solve the problem of insufficient purity of polilidomide, and achieve the effects of environmental friendliness, high yield and easy operation

Inactive Publication Date: 2015-04-29
SHANGHAI INST OF PHARMA IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main problem to be solved by the present invention is to overcome the defect that the purity of polilidomide is not high enough in the existing purification method and provide a kind of purification method of polilidomide

Method used

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  • Method for purifying pomalidomide
  • Method for purifying pomalidomide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The preparation of embodiment 1 polilidomide crude product

[0033] Mix 5 g of 1,3-dioxo-2-(2,6-dioxopiperidin-3-yl)-5-nitroisoindoline and 0.4 g of 10% palladium carbon into 70 mL of N,N - in dimethylacetamide, then carry out hydrogenation reaction at 0.4Mpa, the reaction temperature is 30°C, last 6 hours, filter the catalyst, concentrate the filtrate in vacuo, beat the residue with 40mL water at 40°C overnight, and obtain 3.7g Crude polilidomide as a yellow-green solid. The purity measured by HPLC was 99.0%.

Embodiment 2

[0034] The preparation of embodiment 2 polilidomide crude product

[0035] Mix 5 g of 1,3-dioxo-2-(2,6-dioxopiperidin-3-yl)-5-nitroisoindoline and 0.1 g of 5% palladium carbon into 70 mL of N,N - in dimethylacetamide, then carry out hydrogenation reaction at 0.4Mpa, the reaction temperature is 40°C, last 6 hours, filter the catalyst, concentrate the filtrate in vacuo, beat the residue with 40mL water at 40°C overnight, and obtain 3.7g Crude polilidomide as a yellow-green solid. The purity by HPLC was 95.3%.

Embodiment 3

[0036] The purification of embodiment 3 polilidomide crude product

[0037] Add 1 g of the crude polilidomide in Example 1 to 30 mL of a mixed solvent of N,N-dimethylacetamide and water (the volume ratio of N,N-dimethylacetamide and water is 4:1) and 0.08g of activated carbon, heated to 60°C to dissolve for 1h to 2h, filtered while hot, cooled the filtrate to -10°C, crystallized for 12h, filtered with suction, washed the filter cake with 15mL of water, dried overnight at 40°C to obtain 0.7g poly Pure Methamide. The purity by HPLC was 99.9%.

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Abstract

The invention discloses a method for purifying pomalidomide. The method comprises the following steps: mixing a pomalidomide crude product with high-performance liquid phase purity of 80-90% with a mixed solvent, and crystallizing, wherein the mixed solvent is a mixed solvent of an organic solvent and water; the organic solvent is an amide solvent or a ketone solvent; when the organic solvent is the amide solvent, the volume ratio of the amide solvent to water is 4:1 to 8:1; and when the organic solvent is the ketone solvent, the volume ratio of the ketone solvent to water is 3:1 to 1:3. The purification method disclosed by the invention is simple and convenient to operate, high in yield, high in purity and suitable for the requirements of industrial production regulated by good manufacturing practice.

Description

technical field [0001] The invention relates to a method for purifying polilidomide. Background technique [0002] Pomalidomide, the English name is Pomalidomide, the chemical name is 4-amino-2-(2,6-dioxopiperidin-3-yl)isoindoline-1,3-dione, and its chemical structure is as follows: [0003] [0004] Polidomide is a new immunomodulator originally developed by Celgene. Polidomide is a derivative of thalidomide, which can regulate T cells and inhibit their proliferation, and play an immune regulatory role; by activating natural killer ( natural killer) cells, promote the apoptosis of tumor cells, and are mainly used clinically for the treatment of multiple myeloma. [0005] CN101253163 provides a kind of preparation method of high-purity polilidomide, the mixture of polilidomide crude product and DMSO is put into the reactor, the obtained slurry is heated to 45~50 ℃ and stirred to dissolve until clear, Then rinse with DMSO (400mL), add the solution to purified water (7.2L...

Claims

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Application Information

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IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 刘航袁哲东杨玉雷胡志张颢
Owner SHANGHAI INST OF PHARMA IND
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