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Purification method of argatroban chiral intermediate hydrolysate

A technology of chiral intermediates and purification methods, which is applied in the field of purification of argatroban chiral intermediate hydrolyzate, can solve the problems of high toxicity, difficult recovery, flammability and explosion of acetone, etc., and achieve stable and refined effects Good, environment-friendly effect

Inactive Publication Date: 2016-01-06
天津市亨必达化学合成物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses a large amount of organic solvents methanol and acetone in the refining process, wherein methanol belongs to the second class of solvents, which is highly toxic and environmentally destructive, and acetone is flammable and explosive, has low safety, and is relatively toxic. Miscible, difficult to recycle, causing waste and environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: A kind of purification method of argatroban chiral intermediate hydrolyzate

[0019] Argatroban intermediate hydrolyzate crude product 10 kg, pure water 390 kg, glycerin 0.01 kg, 13X molecular sieve 0.1 kg, mix and stir, heat up to 75°C, keep warm for 30 minutes, filter while hot, filter out 13X type Molecular sieves, the resulting mother liquor was cooled to 0°C for crystallization for 2 hours, filtered, washed with cold water, and dried in the air to obtain the refined product of the hydrolyzate of the argatroban intermediate. The crude hydrolyzate of argatroban intermediate is refined once and characterized by high-performance liquid chromatography. The purity reaches 99.90%, the total impurities can be controlled at no more than 1 / 1000, and the yield is 96.78%.

[0020] The crude argatroban intermediate hydrolyzate in this example was prepared according to the preparation method given in Example 3 in CN201310508082.6, and the 13X molecular sieve was pu...

Embodiment 2

[0021] Embodiment 2: A kind of purification method of argatroban chiral intermediate hydrolyzate

[0022] Argatroban intermediate hydrolyzate crude product 10 kg, pure water 350 kg, glycerin 0.008 kg, 13X molecular sieve 0.08 kg, after mixing, heat up to 65°C under stirring, keep warm for 40 minutes, filter while hot, filter out 13X type molecular sieve, the resulting mother liquor was cooled to -0.5°C and crystallized for 1.5 hours, filtered, washed with cold water, and dried in the air to obtain the refined product of argatroban intermediate hydrolyzate. The crude hydrolyzate of argatroban intermediate is refined once, and characterized by high-performance liquid chromatography, the purity reaches 99.68%, the total impurities can be controlled not higher than 1 / 1000, and the yield is 96.64%.

Embodiment 3

[0024] Embodiment 3: A kind of purification method of argatroban chiral intermediate hydrolyzate

[0025] Argatroban intermediate hydrolyzate crude product 10 kg, pure water 450 kg, glycerin 0.015 kg, 13X molecular sieve 0.2 kg, after mixing, heat up to 80°C with stirring, keep warm for 20 minutes, filter while hot, filter out 13X type molecular sieve, the resulting mother liquor was cooled to 1°C and crystallized for 2.5 hours, filtered, washed with cold water, and dried in the air to obtain the refined product of argatroban intermediate hydrolyzate. The crude argatroban intermediate hydrolyzate is refined once and characterized by high-performance liquid chromatography. The purity reaches 99.78%, the total impurities can be controlled not higher than 1 / 1000, and the yield is 96.23%.

[0026] The crude argatroban intermediate hydrolyzate in this example was prepared according to the preparation method given in Example 3 in CN201310508082.6, and the 13X molecular sieve was pur...

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Abstract

The invention provides a purification method of argatroban chiral intermediate hydrolysate. The purification method comprises the steps of mixing an argatroban chiral intermediate hydrolysate crude product, pure water, glycerol and an adsorbent in proportion, maintaining the temperature at 60-85 DEG C for 20-40 minutes, immediately filtering the adsorbent, carrying out thermal insulation crystallization at (-1)-2 DEG C for 1-5 hours, filtering, flushing with cold water, and airing, so as to obtain an argatroban chiral intermediate hydrolysate finished product. The purification of once finished product is more than or equal to 99.90%, the individual impurity is controlled to be not higher than millesimal, and the industrial mass production is easily realized.

Description

technical field [0001] The invention relates to a method for purifying argatroban chiral intermediate hydrolyzate, which belongs to the field of medicine and chemical industry. Background technique [0002] Argatroban is a new type of thrombin inhibitor that reversibly binds to the active site of thrombin and can be used for anticoagulant therapy in patients with acute ischemic cerebral infarction. For heparin-induced thrombocytopenia and thrombotic syndrome. It has better anticoagulant and antithrombotic effects than heparin, and is the only synthetic drug approved for the treatment of acute ischemic stroke in the world so far. Impurities in drugs may reduce the efficacy of drugs, affect the stability of drugs, and may even cause harm to human health or produce other side effects. Therefore, the removal of impurities in drugs is particularly important. [0003] The existing patent CN201310508082.6 discloses a preparation method of an intermediate of argatroban, wherein th...

Claims

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Application Information

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IPC IPC(8): C07K5/068C07K1/36C07K1/30C07K1/18
Inventor 张智强任晓峰李果王凯宋金津赵钊李连启
Owner 天津市亨必达化学合成物有限公司
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