Method for refining crude lenalidomide product

A technology of lenalidomide and a purification method, which is applied in the field of purification of organic compounds, can solve the problems of low product purity, low yield, low product yield and the like, and achieves high purification yield, high product content, and reduced impurities. The effect of content

Inactive Publication Date: 2013-03-27
NANTONG YUANYA PRECISION MACHINERY
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Problems solved by technology

[0006] Refining method of lenalidomide reported in the literature: China Journal of Pharmaceutical Industry 2008.39 (12) Fang Feng et al. reported in the literature on the synthesis of lenalidomide that the crude product was washed with water, and the purity of the obtained product was not high, and the yield was low. The yield was 76%
Chinese Journal of Pharmaceutical Industry 2010.41 (3) Wu Han and others reported in the synthesis literature of lenalidomide that extraction with dichloromethane, drying and filtration over anhydrous sodium sulfate, distillation under reduced pressure, and drying resulted in low product yields. 69%

Method used

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Embodiment Construction

[0018] 1. The comparative example is the existing method for purifying crude lenalidomide: add 10.0 g of crude lenalidomide, acetone: water (1:1) 300 mL into the reaction bottle, and heat up until the crude lenalidomide solids are completely dissolved Finally, add an appropriate amount of activated carbon, keep warm for 30 minutes, heat filter, the filtrate cools down and crystallizes, naturally cools down to room temperature, keeps warm at 0~5°C for 2 hours, filters with suction, washes the filter cake with cold acetone, and dries the filter cake at room temperature under reduced pressure to produce a white solid 6.9 g, 69% yield, 95.0% purity as measured by HPLC (High Performance Liquid Chromatography).

[0019] 2. Add 10.0g of crude lenalidomide, 300mL of isopropanol: water (1:1) into the reaction bottle, raise the temperature until the crude solid of lenalidomide is completely dissolved, then add 5g of activated carbon and 0.5g of nano-ceramic powder, Keep warm for 30 minu...

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Abstract

The invention discloses a method for refining a crude lenalidomide product. The method comprises the following steps of: (1) adding the crude lenalidomide product to a mixed solution of isopropanol and water; (2) heating, after the crude lenalidomide product is completely dissolved, adding activated carbon and nanometer ceramic powder and carrying out heat preservation for the first time; (3) filtering when the solution is hot, and cooling filtrate till crystals precipitate; and (4) carrying out heat preservation for the second time, carrying out suction filtering after the crystal precipitation is finished, and finally drying. Due to adoption of the technical scheme, the method for refining the crude lenalidomide product has the beneficial effects of low isopropanol toxicity, high safety, simpleness in process, no need of special equipment and environment requirements, suitability for industrial production, high product content and high refining yield; and the purify of the lenalidomide is remarkably improved.

Description

technical field [0001] The invention belongs to the technical field of purification of organic compounds, in particular to a method for refining crude lenalidomide. Background technique [0002] The chemical name of lenalidomide is 3-(4-amino-1-oxo-1,3-dihydro-isoindol-2-yl)piperidine-2,6-dione, and its chemical structural formula is, , In 2008, the U.S. Food and Drug Administration (FDA) approved a new indication of lenalidomide from American Cell Gene Company, which is combined with dexamethasone (Dexamethasone) to treat multiple myeloma who have received at least one therapy patient. [0003] Lenalidomide is a new generation of antineoplastic drug developed by Celgene in the United States. Its active ingredient is lenalidomide, which is mainly used for the treatment of chronic myeloma and myelodysplastic syndrome (MDS) with 5q deletion. . Lenalidomide is a new generation derivative of thalidomide, but it has not been found to have mutagenic toxicity, and its efficacy ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
Inventor 张华
Owner NANTONG YUANYA PRECISION MACHINERY
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