Method for purifying orlistat intermediate

A statin, medium technology, applied in the field of medicine, can solve the problems of high equipment requirements, long production cycle, high production cost, etc., and achieve the effect of less capital required for equipment, low equipment requirements, and low toxicity

Active Publication Date: 2013-12-04
HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The present invention aims at the disadvantages of low yield, complex process, long production cycle, high equipment requirements, large amount of solvent, high production cost, and difficult scale-up in the prior art for purifying primastatin, and provides a hi

Method used

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  • Method for purifying orlistat intermediate
  • Method for purifying orlistat intermediate
  • Method for purifying orlistat intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1) Fermentation broth pretreatment: take 5t of freshly cultivated liprestatin fermentation broth, add 150kg of filter aid magnesium oxide, 2.8kg of flocculant ferric chloride, adjust the pH to 4.0 with hydrochloric acid, and filter with plate and frame to obtain 1t containing A mixture of liprestatins.

[0053] 2) Extraction: Add the liprestatin-containing mixture into 6000L isopropanol solution for microbial cell disruption, stir for 1 hour, and plate-frame filter to obtain an extract containing liprestatin.

[0054] 3) Phase inversion:

[0055] Phase inversion for the first time: add 3600L of drinking water and 3600L of petroleum ether to the leaching solution, stir for 10 minutes, then let stand for 1 hour to separate layers, and take the upper petroleum ether phase;

[0056] The second phase inversion: add 2160L isopropanol to the petroleum ether phase, stir for 5 minutes and let it stand for 1 hour to separate the layers. Use TLC to spot the isopropanol phase to j...

Embodiment 2

[0059] 1) Fermentation broth pretreatment: Take 5t of freshly cultivated liprestatin fermentation broth, add 200kg of filter aid perlite, 500ml of flocculant polyacrylamide, adjust the pH to 3.5 with hydrochloric acid, and filter with plate and frame to obtain 1t of liprestatin containing A mixture of statins.

[0060] 2) Extraction: add the liprestatin-containing mixture into 4000L ethanol solution for microbial cell disruption, stir for 1 hour, and plate-frame filter to obtain the liprestatin-containing mixture extract.

[0061] 3) Phase inversion:

[0062] Phase inversion for the first time: add 2000L drinking water and 2000L heptane to the extract solution, stir for 10 minutes, then let stand for 1 hour to separate layers, and take the upper heptane phase;

[0063] The second phase inversion: add 1000L acetonitrile to the heptane phase, stir for 5 minutes and let it stand for 1 hour to separate the layers. Use TLC to spot the acetonitrile phase to judge the effect of remo...

Embodiment 3

[0066] 1) Fermentation broth pretreatment: Take 5t of freshly cultivated liprestatin fermentation broth, add 200kg of filter aid cellulose, 0.5kg of flocculant polymerized aluminum iron silicate, adjust the pH to 6.0 with hydrochloric acid, and filter with plate and frame to obtain 1t A mixture containing liprestatin.

[0067] 2) Extraction: Add the mixture containing riprestatin to 4000L isopropanol solution for microbial cell disruption, stir for 1 hour, and filter with a plate frame to obtain an extract of the mixture containing riprestatin.

[0068] 3) Phase inversion:

[0069] Phase inversion for the first time: add 2400L drinking water and 2000L n-hexane to the extract solution, stir for 10 minutes, then let stand for 1 hour to separate layers, and take the upper n-hexane phase;

[0070] Wash with water to remove impurities: add 600L of drinking water to the n-hexane phase, stir for 5 minutes, let stand for 1 hour to separate layers, and take the upper n-hexane phase; ...

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Abstract

The invention belongs to the technical field of medicine and particularly relates to a method for purifying the important intermediate lipstatin of orlistat serving as a weight-reducing aid. The method provided by the invention comprises fermentation liquor pretreatment, extracting, phase inversion and concentration. The product obtained by using the method is high in purity, and the process provided has the advantages of high yield, short period, simplicity and easiness in control, less equipment menstruum investment and low production cost, and is very suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for purifying liprestatin, an important intermediate of weight-loss drug orlistat. technical background [0002] Lipstatin is refined from Streptomyces tocytricini through biological fermentation and solvent extraction. It is a new pancreatic lipase inhibitor that can selectively inhibit pancreatic lipase in the gastrointestinal tract. , Reduce the decomposition and absorption of fat. Its tetrahydro derivatives have been successfully developed by the Swiss company Roche as Xenical, also known as Orlistat, which is currently the only drug that treats obesity through non-central nervous system effects. [0003] Lipstatin (lipstatin) is an important intermediate of weight loss drug orlistat, and its structural formula is: [0004] [0005] There are two ways to prepare Orlistat: total synthesis and semi-synthesis. Most of the orlistat APIs currently used clinically are ...

Claims

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Application Information

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IPC IPC(8): C07D305/12
Inventor 李宏杰方军蒋彩霞沈康刘金国吴国勇
Owner HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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