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Preparation method for high-purity pomalidomide

A kind of pomalidomide, high-purity technology, applied in the preparation field of high-purity pomalidomide, can solve the problems such as raw material I difficult to react completely, the amount of solvent is large, the yield is low, etc., achieves good inhibitory effect, solvent usage The effect of less and high conversion rate of raw materials

Active Publication Date: 2017-04-19
YANGTZE RIVER PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Wu Gang (Chinese Journal of Medicinal Chemistry, 2013 (2), 108-110) reported that using methanol as a solvent, palladium carbon-ammonium formate system reduction to obtain pomalidomide, the disadvantage of this method is that the amount of solvent required is large, and the raw material I is difficult to react completely, and yield is lower (68% of bibliography report)

Method used

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  • Preparation method for high-purity pomalidomide
  • Preparation method for high-purity pomalidomide
  • Preparation method for high-purity pomalidomide

Examples

Experimental program
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Effect test

Embodiment 1

[0054] (1) Add 100g 3-nitro-N-(2,6-dioxo-3-piperidinyl)phthalimide, 10g palladium carbon and 1000ml N-methylpyrrolidone to a 2000ml hydrogenation reactor In the middle, vacuumize, replace with nitrogen for 3 times, then pass in hydrogen, adjust the pressure in the kettle to 0.3Mpa, control the temperature at 45°C, after the reaction is complete, filter with suction, add 30g of medicinal charcoal to the filtrate, heat up to 70°C, and stir for 3 hours. Suction filtration;

[0055] (2) Add the aqueous solution of sodium carbonate (2g sodium carbonate is dissolved in 10ml purified water to make) in step (1) last gained filtrate, stir at room temperature for 0.5 hour, then slowly add dropwise 2000ml purified water, cool to 10 ℃ of crystallization, Suction filtration, the resulting filter cake was added to 500ml of purified water, stirred at room temperature for 0.5 hours, suction filtration, the filter cake was washed with purified water, and the solid was vacuum-dried at 60°C to o...

Embodiment 2

[0057] (1) Add 100g 3-nitro-N-(2,6-dioxo-3-piperidinyl)phthalimide, 10g palladium carbon and 1200ml N-methylpyrrolidone to a 2000ml hydrogenation reactor In the middle, vacuumize, replace with nitrogen for 3 times, then pass in hydrogen, adjust the pressure in the kettle to 0.5Mpa, control the temperature at 50°C, after the reaction is complete, filter with suction, add 30g of medicinal charcoal to the filtrate, heat up to 70°C, and stir for 3 hours. Suction filtration;

[0058] (2) Add an aqueous solution of potassium carbonate (3g of potassium carbonate is dissolved in 12ml of purified water) to the final filtrate of step (1), stir at room temperature for 0.5 hour, then slowly add 2000ml of purified water dropwise, cool to 10°C for crystallization, Suction filtration, the resulting filter cake was added to 500ml of purified water, stirred at room temperature for 0.5 hours, suction filtration, the filter cake was washed with purified water, and the solid was vacuum-dried at 6...

Embodiment 3

[0060] (1) Add 100g 3-nitro-N-(2,6-dioxo-3-piperidinyl)phthalimide, 12g palladium carbon and 1200ml N-methylpyrrolidone to a 2000ml hydrogenation reactor In the process, vacuumize, replace nitrogen for 3 times and then pass in hydrogen, adjust the pressure in the kettle to 0.5Mpa, control the temperature at 50°C, after the reaction is complete, filter with suction, add 30g of medicinal charcoal to the filtrate, heat up to 70°C, and stir for 6 hours. Suction filtration;

[0061] (2) Add an aqueous solution of sodium carbonate (2g sodium carbonate is dissolved in 12ml purified water to make) in step (1) last gained filtrate, stir at room temperature for 0.5 hour, then slowly add dropwise 2000ml purified water, cool to 10 ℃ of crystallization, Suction filtration, the resulting filter cake was added to 500ml of purified water, stirred at room temperature for 0.5 hours, suction filtration, the filter cake was washed with purified water, and the solid was vacuum-dried at 70°C to obt...

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Abstract

A preparation method for high-purity pomalidomide comprises the following steps: (1) adding 3-nitro-N-(2,6-dioxo-3-piperidyl)phthalimide, palladium carbon and N-methyl pyrrolidone to a reaction kettle, vacuumizing, then introducing hydrogen gas, carrying out suction filtration after a reaction is complete, adding medicinal charcoal to the filtrate, stirring, heating, and carrying out suction filtration; and (2) adding an alkaline aqueous solution to the filtrate finally obtained in the step (1), stirring, then adding purified water, cooling and crystallizing, carrying out suction filtration, adding purified water to the obtained filter cake, stirring, carrying out suction filtration, washing, and drying to obtain the high-purity pomalidomide product. The preparation method provided by the invention has the advantages of simple operation and mature and stable technology, and can significantly improve the quality of pomalidomide; the purity of the obtained product is greater than 99.5%, the contents of single impurities are all less than 0.1%, and the medicinal requirements are met.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of high-purity pomalidomide. Background technique [0002] Pomalidomide (Pomalidomide) was developed by Celgene Corporation of the United States. It was approved by FDA in February 2013 and approved by EMA in August 2013. Pomalidomide is the third new immunomodulator after thalidomide and lenalidomide. It has anti-tumor activity and can inhibit the proliferation of hematopoietic tumor cells and induce apoptosis. Pomalidomide is clinically used to treat multiple myeloma ineffective by other drugs (such as lenalidomide and bortezomib), and has huge market potential. [0003] The chemical name of pomalidomide is 3-amino-N-(2,6-dioxo-3-piperidinyl)phthalimide, and its structural formula is as follows: [0004] [0005] There are many preparation methods about pomalidomide, but the preparation method commonly used at present is from 3-nitro-N-(2,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 梁慧兴孙伟翟佳平张利军尹利献黄猛张海波陈令武
Owner YANGTZE RIVER PHARM GRP CO LTD
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