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Purification method of zaltoprofen

A purification method and molecular sieve technology are applied in the field of preparation of high-purity zaltoprofen, which can solve the problems of poor safety, large production limitations, large amount of solvent used, etc. Effect

Inactive Publication Date: 2015-12-30
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

[0004] In summary, the currently reported refining process has the following problems: the purity of the purified product needs to be further improved in one-time refining, and usually the purity of zaltoprofen cannot be increased to more than 99.95% even after repeated refining, and the yield of crystallization and purification operations is generally low. Moreover, the refined crystallization solvents used are ethylene dichloride, methanol, and acetone, which are highly toxic or regulated precursor solvents. The production limitations are large and the safety is poor. At present, no adsorbent is used, so the amount of solvent used is also low. It is relatively large, and it is difficult to reach the industrial production level of 100 kilograms. The organic solvent used in the traditional recrystallization process is highly flammable and explosive, and has good water solubility. environmental phenomenon

Method used

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  • Purification method of zaltoprofen

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Experimental program
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Effect test

Embodiment 1

[0016] 100 kg of Zaltobuprofen crude product, 400 kg of ethyl acetate, 200 kg of isopropyl acetate, 2 kg of molecular sieve (type 5A molecular sieve, 8x12 mesh, Shanghai Youxin Molecular Sieve Co., Ltd.), mix and heat up to 53 ℃, heat preservation for 90 minutes, filter while it is hot, filter out molecular sieves, cool the obtained mother liquor to -3 ℃ and crystallize for 90 minutes, filter, and dry in the air to obtain zaltoprofen refined and purified product, the purity determined by HPLC is 99.97%, the total product The rate is 96.7%. HPLC assay results see figure 1 .

Embodiment 2

[0019] 100 kg of Zaltobuprofen crude product, 300 kg of ethyl acetate, 100 kg of isopropyl acetate, 1 kg of molecular sieve, mixed and stirred, heated to 53°C, kept for 90 minutes, filtered while hot, filtered out molecular sieve, obtained The mother liquor was cooled to -3°C and crystallized for 90 minutes, filtered, and dried to obtain a refined zaltoprofen product with a purity of 99.96% as determined by HPLC and a total yield of 95.7%.

[0020] The crude product of zaltoprofen in this example is prepared according to the method provided in Example 2 of CN200910067886.0.

Embodiment 3

[0022] 100 kg of Zaltobuprofen crude product, 500 kg of ethyl acetate, 300 kg of isopropyl acetate, 3 kg of molecular sieve, mixed and stirred, heated to 53 ° C, kept for 90 minutes, filtered while hot, filtered out molecular sieve, obtained The mother liquor was cooled to -3°C and crystallized for 90 minutes, filtered, and dried to obtain a refined product of zaltoprofen. The purity determined by HPLC was 99.95%, and the total yield was 95.9%.

[0023] The crude product of zaltoprofen in this example is prepared according to the method provided in Example 2 of CN200910067886.0.

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Abstract

The invention relates to a purification method of zaltoprofen. A zaltoprofen crude product, ethyl acetate, isopropyl acetate and molecular sieves are mixed and are kept at the temperature ranging from 51 DEG C to 55 DEG C for 80-100 minutes, the molecular sieves are screened out, then a mother solution is naturally cooled and is kept at the temperature ranging from subzero 4 DEG C to subzero 2 DEG C, crystalized for 2-3 hours, filtered and aired, and the refined and purified zaltoprofen is prepared. With the adoption of the refining and purification method, the purity of zaltoprofen can be 99.95% or higher after the zaltoprofen crude product is refined once, the total impurity rate can be controlled to be under five in ten thousand, the yield is higher than 95%, and the yield per unit can reach the quintal-level industrial production. A low-toxicity environment-friendly reagent is used for crystallization, solvents can be completely recycled and are low in price, no environment pollution is caused, and operation is facilitated.

Description

technical field [0001] The invention relates to a preparation of high-purity zaltoprofen, in particular to a method for purifying zaltoprofen. Background technique [0002] Zaltoprofen, whose chemical name is 2-(10,11-dihydro-10-oxodibenzo[b,f]thiazem-2-yl)propanoic acid, is an anti-inflammatory, analgesic, Non-steroidal anti-inflammatory drug with antipyretic effect, it mainly works by inhibiting the synthesis of prostaglandins and blocking inflammatory mediators, it is clinically used to treat chronic rheumatoid arthritis, osteoarthritis, low back pain, shoulder joint Anti-inflammatory analgesia for inflammation, neck-shoulder-wrist syndrome, surgery, trauma, and tooth extraction. [0003] Chinese patents CN201410287231.5, CN201380010158.0 and CN200910067886.0 all disclose a preparation method of zaltobuprofen. In the CN200910067886.0 method, the synthetic Zaltoprofen crude product is recrystallized and purified with anhydrous methanol or ethanol, and the yield is 84.5% ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D337/14
CPCY02P20/582C07D337/14
Inventor 张智强任晓峰李静雅张宁宋金津李果吴海明赵钊韩瑞婷赵颖王凯
Owner 天津药物研究院药业有限责任公司