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Method for refining argatroban refining mother liquor recycling product

A mother liquor recovery and argatroban technology, which is applied in the preparation methods of peptides, chemical instruments and methods, organic chemistry, etc., can solve the problems of inability to purify the mother liquor recovered products, so as to reduce production costs, increase economic benefits, and improve Effect of Refinement Rate

Active Publication Date: 2015-04-29
天津药物研究院药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, can't refine mother liquor recovery product by existing method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Put 10.0g of recovered argatroban refined mother liquor and 30.0mL of absolute ethanol into the reaction bottle, heat and reflux for 5 minutes, then add 0.5g of neutral alumina and 0.5g of silica gel after cooling down slightly, heat and reflux for 5 minutes, heat Filtration, the filtrate was crystallized at 0°C for 10 hours, filtered, and dried to obtain 4.2 g of the primary refined product of the recovered argatroban mother liquor, with a yield of 42.0%.

[0022] 2) Put 5.0g of the primary refined product of the recovered argatroban mother liquor into the reaction bottle, then add 25mL of 95% ethanol and 0.5g of activated carbon, reflux for 5 minutes, heat filter, and crystallize the filtrate at 0°C for 10 hours, filter and dry , to obtain 3.5g of argatroban fine product, yield 70%, related substances: main peak 99.70%, maximum simple impurities 0.08%.

Embodiment 2

[0024] 1) Put 10.0g of recovered argatroban refined mother liquor and 50.0mL of absolute ethanol into the reaction bottle, heat and reflux for 5 minutes, then add 5.0g of neutral alumina and 5.0g of silica gel after cooling down slightly, heat and reflux for 5 minutes, heat After filtration, the filtrate was crystallized at 10°C for 10 hours, filtered, and dried to obtain 3.5 g of a primary refined product of the recovered product of argatroban mother liquor, with a yield of 35.0%.

[0025] 2) Put 5.0g of the primary refined product of the recovered argatroban mother liquor into the reaction bottle, then add 25mL of 95% ethanol and 0.5g of activated carbon, reflux for 5 minutes, heat filter, and crystallize the filtrate at 0°C for 10 hours, filter and dry , 3.7g of fine argatroban was obtained, with a yield of 74.0%, related substances: main peak 99.88%, maximum single impurity 0.04%.

Embodiment 3

[0027] 1) Put 10.0g of recovered argatroban refined mother liquor and 100.0mL of absolute ethanol into the reaction bottle, heat and reflux for 5 minutes, then add 5.0g of neutral alumina and 10.0g of silica gel after cooling down slightly, heat and reflux for 5 minutes, heat After filtering, the filtrate was crystallized at 10°C for 10 hours, filtered, and dried to obtain 2.2 g of a primary refined product of the recovered product of argatroban mother liquor, with a yield of 22.0%.

[0028] 2) Put 5.0g of the primary refined product of the recovered argatroban mother liquor into the reaction bottle, then add 25mL of 95% ethanol and 0.5g of activated carbon, reflux for 5 minutes, heat filter, and crystallize the filtrate at 0°C for 10 hours, filter and dry , to obtain 3.4g of argatroban fine product, yield 68.0%, related substances: main peak 99.91%, maximum simple impurities 0.04%.

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Abstract

The invention discloses a method for refining an argatroban refining mother liquor recycling product. The method comprises the following steps: adding the argatroban refining mother liquor recycling product and absolute ethyl alcohol to a reaction bottle; heating, refluxing, and dissolving, slightly cooling, adding neutral alumina and silica gel as adsorbents; carrying out hot filtration, cooling filtrate, devitrifying, filtering and drying to obtain a primary refined product of the argatroban refining mother liquor recycling product; feeding the argatroban refining mother liquor recycling product to the reaction bottle, adding 5fold of 95% (W / V) ethanol and 0.1fold of activated carbon, refluxing for 5-10 hours and carrying out hot filtration; and devitrifying the filtrate at 0-25 DEG C for 10-12 hours, filtering and drying to obtain an argatroban refined product. The method is simple to operate; the argatroban refining rate is increased; and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical synthesis chemistry, in particular to a method for refining argatroban refined mother liquor recovery product. Background technique [0002] Argatroban is a low-molecular-weight thrombin inhibitor derived from L-arginine, and it is the only synthetic drug approved for the treatment of acute ischemic stroke in the world so far. In 1978, Mitsubishi Chemical Company of Japan reported the antithrombin activity of argatroban monohydrate for the first time, and it was used for the clinical treatment of peripheral arterial occlusive disease, and then for the treatment of arterial thrombosis. It was approved by the United States in 2000. Addtroban is used to treat HIT patients. In 2002, FDA approved argatroban for anticoagulant treatment of HIT patients requiring interventional therapy. In recent years, with the introduction of the concept of acute coronary syndrome (acllte coronary syndrome, ACs)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/068C07K1/14
Inventor 汪洋张宁张士欣王悦伟
Owner 天津药物研究院药业有限责任公司
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