Method for purifying orlistat

A technology for orlistat and samples, which is applied in the field of preparing high-purity orlistat, and can solve problems such as inability to purify orlistat

Active Publication Date: 2006-04-26
HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention overcomes the defect that low-purity orlistat cannot be purified in the prior art, and provides a purification method that can purify low-purity orlistat to meet pharmaceutical standards and is suitable for industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The fermentation extract concentrate contains lipstatin 30% (w / w) 120ml, and the sample is obtained after hydrogenation. It contains 46g orlistat sample, the content is 52%, and the sample color is about gray. Add 150ml of acetone to dissolve and filter, and add acetone to 600ml. After crystallization and suction filtration, 30 g of crystals were obtained, which was off-white, with a content of 96% (W / W) detected by HPLC, and the maximum impurity was 0.52%. Then add 120ml of acetone, dissolve, filter, add acetone to 400ml, crystallize at low temperature, and filter with suction to obtain 25g of crystals, off-white, detected by HPLC, content 97%, maximum impurity 0.4%. Add 500ml heptane to re-dissolve, filter, add heptane to 900ml, and crystallize to obtain 20g of orlistat pure product with a content of 98.8% and a maximum impurity of 0.4%.

Embodiment 2

[0029] The purity of the fermentation extract concentrate Lipstatin is 40% (weight / weight) 90ml, and the HPLC purity is 74% (calculated by the peak area normalization method). After hydrogenation, 52g of orlistat sample is obtained, the content is 68.9%, and the maximum impurity is 2.0%. 110ml of ethanol was dissolved, filtered, and supplemented with ethanol to 530ml, and crystallized to obtain 35g of orlistat sample with a purity of 83.1% and a maximum impurity of 0.9%. Add 550ml of heptane to re-dissolve, filter, add heptane to 1300ml, and crystallize to obtain 34g of orlistat sample with a purity of 88.1% and a maximum impurity of 0.9%. Add 700ml of heptane to re-dissolve, filter, add heptane to 1000ml, and crystallize to obtain 14g of orlistat pure product with a purity of 98.5% and the maximum impurity less than 0.5%.

Embodiment 3

[0031]The fermentation extract concentrate contains 100ml of lipstatin 35% (weight / weight), HPLC purity 71% (calculated by the peak area normalization method), after hydrogenation, about 51g of orlistat sample is obtained, the content is 70%, the sample color is gray, add 150ml of acetonitrile was dissolved, filtered, acetonitrile was added to 750ml, and crystallized to obtain 32g of orlistat sample, off-white, purity 91.1%, maximum impurity 0.92%; add 750ml of hexane to re-dissolve, filter, add hexane to 1400ml, Crystallized to obtain 31 g of orlistat sample with a purity of 93.5% and a maximum impurity of 0.92%. Add acetonitrile 65mi to dissolve, filter, add acetonitrile to 310mi, crystallize to obtain 18g of orlistat sample, off-white, purity 95.1%, maximum impurity 0.53%; add 270ml of hexane to redissolve, filter, add hexane to 420ml , Crystallized to obtain 16 g of orlistat pure product with a purity of 98.6% and a maximum impurity of less than 0.5%.

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Abstract

The present invention discloses orlistat purifying method, which includes dissolving coarse orlistate product in medium polarity solvent, filtering, eliminating impurity, crystallization, dissolving in non-polar solvent, recrystallization, and repeating some steps until reaching the medicinal purity standard. The said method is suitable for purifying coarse orlistate product with purity of 50-85 %, and has the advantages of high yield, short purification period, simple purification process and being suitable for industrial production.

Description

Technical field [0001] The present invention relates to a method for purifying organic compounds. Specifically, the present invention relates to a method for preparing high-purity orlistat. Background technique [0002] Orlistat is a hydrogenated derivative of the natural product of Streptomyces lipstatin (nipostatin), and its chemical name is (S)-2-formylamino-4-methyl-valerate ( S)-1-[[(2S, 3S,)-3-hexyl-4-oxo-2-oxetanyl]-methyl]-dodecyl ester. Orlistat is a specific gastrointestinal lipase inhibitor used to prevent and treat obesity-related diseases. [0003] The Chinese patent "Method for Purification of Pancreatin" (Publication No.: CN1266058A, published on September 13, 2000), discloses a method for purifying orlistat, which uses heptane for the lipatatin produced by the fermentation of Streptomyces Two-stream extraction is carried out with aqueous acetic acid, and hexane or heptane is used for hydrogenation and crystallization. The US patent leucine derivatives (patent numb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/12
Inventor 朱健陈晓霞
Owner HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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