Method for preparing orlistat

A technology for orlistat and statin, applied in the field of extraction and purification of orlistat, can solve the problems of complex process steps, difficulty in obtaining high purity and the like

Active Publication Date: 2011-01-19
鲁南新时代生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention overcomes the defects of complicated process steps and difficulty in obtaining high-purity orlistat in the prior art, removes highly polar impurities through macroporous adsorption resin, and removes impurities with similar structures to orlistat through silica gel column chromatography , providing a method for preparing orlistat into a high-purity pharmaceutical product and suitable for industrial production

Method used

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  • Method for preparing orlistat

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Effect test

Embodiment 1

[0024] Add 100 liters of acetone to 100 liters of orlistat intermediate nipostatin fermentation broth (fermentation unit: 7 g / liter), stir and extract for 1 hour, and filter by plate and frame to obtain 190 liters of acetone extract. Filter through a titanium rod filter, adjust the pH to 3.0 with oxalic acid after filtration, and pack 20 liters of HZ820 macroporous adsorption resin into a column to absorb the acetone leaching solution after pretreatment, and the adsorption speed is 10 liters / hour. After the adsorption was completed, 60 liters of 80% acetone solution was used to elute, and the elution speed was 16 liters / hour, and the acetone eluate containing nipostatin was collected by TLC detection. After the elution was completed, 60 liters of acetone eluent containing nipostatin was obtained.

[0025] Add 20 liters of water to 60 liters of acetone eluent, adjust the acetone concentration to about 60%, add 20 liters of heptane for extraction, and after extraction for 1 hour...

Embodiment 2

[0030] After 500 liters of nipostatin fermentation broth (fermentation unit 7.2 g / liter) was stirred and leached with 750 liters of acetone for 1 hour, the plate and frame were filtered to obtain 1200 liters of acetone leaching solution, which was then filtered with a 0.1um titanium rod filter. After filtration, the pH was adjusted to 4.0 with oxalic acid, and 90 liters of HZ820 macroporous adsorption resin was packed into a column to absorb the acetone leaching solution after pretreatment, and the adsorption speed was 50 liters / hour. After adsorption, 350 liters of 80% acetone solution was used to elute, and the elution speed was 90 liters / hour, and the acetone eluate containing nipostatin was collected by TLC detection. After elution, 350 liters of acetone eluent containing nipostatin were obtained.

[0031] Add 118 liters of water to 340 liters of acetone eluent, adjust the acetone concentration to about 65%, add 120 liters of heptane for extraction for 1 hour, statically s...

Embodiment 3

[0036]Add 1,400 liters of acetone to 1,000 liters of nipostatin fermentation broth (fermentation unit 6.6 g / liter), and then add 1,400 liters of acetone to stir and extract for 1 hour, then filter to obtain 2,200 liters of acetone extract. Adjust the pH to 4.5, 160 liters of HZ818 macroporous adsorption resin is packed into a column, and after pretreatment, the acetone leaching solution is adsorbed at a speed of 80 liters / hour. liter / hour, and the acetone eluate containing nipostatin was collected by TLC detection. After the elution was completed, 640 liters of acetone eluent containing nipostatin were obtained.

[0037] Add 210 liters of water to 640 liters of acetone eluent, adjust the acetone concentration to about 60%, add 220 liters of heptane for extraction for 1 hour, statically separate layers, and concentrate the heptane extraction phase to obtain 8.95 kg of crude nipostatin, of which nipostatin The statin concentration was 58%.

[0038] 8.95 kg of crude nipostatin ...

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Abstract

The invention belongs to the technical field of medicaments, and particularly relates to a novel method for preparing weight-losing medicament orlistat by a fermentation method. The method for preparing the orlistat comprises the following steps of: extraction and filtering of fermentation solution, chromatographic impurity removal by macroporous absorption resin, silica column chromatography of orlistat after hydrogenation and the like. By method, the effects of better removing impurities and purifying products are achieved.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for producing orlistat, in particular to a new method for extracting and purifying orlistat. Background technique [0002] Orlistat is a long-acting and potent specific inhibitor of gastrointestinal lipase, which acts by inactivating the enzyme by forming a covalent bond with the active serine site of gastric lipase and pancreatic lipase in the lumen of the stomach and small intestine It is mainly used for the treatment and prevention of obesity-related disorders. Its chemical name is: (S)-2-formamido-4-methyl-valerate (S)-1-[[(2S,3S)-3-hexyl-4-oxo-2-oxo heterocycle Butyl] methyl]-dodecyl ester, the structural formula is as follows: [0003] [0004] Orlistat can be produced by total synthetic methods as well as fermentation methods. The production method of orlistat involved in this patent is fermentation production, which is a hydrogenated derivative of nipostatin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/12
Inventor 赵志全刘茂田
Owner 鲁南新时代生物技术有限公司
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