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Preparation method of orlistat

A technology of orlistat and preparation column, applied in the direction of organic chemistry, etc., can solve problems such as the simplicity of operation steps, amplification linearity and yield, and no significant breakthrough in purification process, so as to achieve easy production control, reduce Effects of solvent consumption and shortened production cycle

Active Publication Date: 2012-09-26
ZHUHAI UNITED LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent application with the publication number CN101948450A and the title of the invention "A Method for the Production and Preparation of Orlistat" still adopts the combination of ordinary silica gel column and repeated crystallization for purification. still need to be further improved
[0008] In addition, there are also preparation methods that combine extraction, cooling crystallization, extraction, adsorption filtration and vacuum drying, as described in patents such as WO2005 / 007639, WO2005 / 026140, and WO2009 / 040827. These patent applications are still in the Roche patent to a certain extent. Partial improvement on the basis of technology, no significant breakthrough in purification process

Method used

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  • Preparation method of orlistat
  • Preparation method of orlistat
  • Preparation method of orlistat

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Mix about 80Kg with a particle size of 10μm and a pore size of Pour the reversed-phase C18 spherical silica gel filler into about 150L of isopropanol, stir evenly to make a filler slurry, remove filler fragments and fine powder, quickly pour it into a DAC preparation column with an inner diameter of φ800mm, and set the column packing pressure to 20MPa , Open the pneumatic piston rod of the column packing machine for axial compression, and at the same time open the valve at the lower end of the DAC preparation column to discharge and recover the isopropanol. When the piston is compressed to the set pressure of 20MPa, the column packing is completed, the height of the column bed is 250mm, and the specification of the column bed is φ800mm×250mm. The installed DAC preparative column has been tested for column efficiency, and the number of theoretical plates reaches 46812N / m.

[0043] Liprestatin (purity 87.46%, content 66.20%) was dissolved in 86% methanol solution, and t...

Embodiment 2

[0049] Mix about 75Kg with a particle size of 10μm and a pore size of Pour the reversed-phase C8 spherical silica gel filler into about 150L of isopropanol, stir evenly to make a filler slurry, remove filler fragments and fine powder, and quickly pour it into a DAC preparation column with an inner diameter of φ800mm, and set the column packing pressure to 24MPa , Open the pneumatic piston rod of the column packing machine for axial compression, and at the same time open the valve at the lower end of the DAC preparation column to discharge and recover the isopropanol. When the piston is compressed to the set pressure of 24MPa, the column packing is completed, the height of the column bed is 250mm, and the specification of the column bed is φ800mm×250mm. The installed DAC preparative column has been tested for column efficiency, and the number of theoretical plates reaches 42663N / m.

[0050] Liplastatin (purity 87.46%, content 66.20%) was dissolved in 85% methanol solution, th...

Embodiment 3

[0055] Mix about 10Kg with a particle size of 15 μm and a pore size of Pour high-pressure resistant reverse-phase polymer resin filler based on polystyrene / divinylbenzene into about 20L of isopropanol, stir evenly to make filler slurry, remove filler fragments and fine powder, and pour it quickly to an inner diameter of φ300mm In the DAC preparation column cylinder, set the pressure to 10MPa, open the pneumatic piston rod of the column packing machine to perform axial compression, and simultaneously open the valve at the lower end of the DAC preparation column to discharge and recover the isopropanol. When the piston is compressed to the set pressure of 10MPa, the column packing is completed, the height of the column bed is 300mm, and the specification of the column bed is φ300mm×300mm. The installed DAC preparative column has been tested for column efficiency, and the number of theoretical plates reaches 38764N / m.

[0056] Liprestatin (purity: 89.17%, content: 64.56%) was d...

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Abstract

The invention discloses a preparation method of orlistat, which comprises the following steps: (1) using reverse phase silica gel or reverse phase polymer resin as a filler of a DAC (dynamic axial compression) preparative column, and uniformly mixing an organic solvent and the filler to prepare a slurry; (2) filling the filler slurry into a cylinder of the DAC preparative column, and starting a column packing machine to carry out axial compression; (3) pumping a mobile phase into the DAC preparative column by using a preparative pump, thereby carrying out displacement washing on the organic solvent in the column and balancing the preparative column; (4) injecting a crude orlistat product solution into the DAC preparative column by using a high-pressure preparative pump to carry out columnadsorption; (5) after the column adsorption, analyzing the orlistat solution by using a mobile phase, and collecting the analytic liquid in multiple sections; and (6) merging samples with qualified purity, concentrating, crystallizing and drying to obtain the finished orlistat product. By using the purification and preparation method of orlistat researched and developed by the invention, the purification and preparation amount of orlistat per batch is up to several kilograms and even myriagrams, and the purification production cycle is shortened to about 1-2 hours from tens of hours in the past.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy and relates to a method for purifying and preparing organic compounds. Specifically, the invention relates to a method for preparing a high-purity lipase inhibitor orlistat. technical background [0002] Orlistat (Orlistat) is a derivative obtained by catalytic hydrogenation of the secondary metabolite lipstatin (lipstatin) fermented by the actinomycete Streptomyces toxytricini, so it is also called tetrahydroliprex Statin (Tetrahydrolipstatin, THL), chemical name N-formyl-L-leucine (1S)-1-[[(2S,3S)-3-hexyl-4-oxo-oxetanyl]methyl] Lauryl ester or (S)-2-formamido-4-methyl-pentanoic acid (S)-1-[[(2S,3S)-3-hexyl-4-oxo-oxetane base] methyl] dodecyl ester. The chemical reaction formula of lipstatin (lipstatin) to generate orlistat (Orlistat) after catalytic hydrogenation is as follows: [0003] [0004] Orlistat is a specific gastrointestinal lipase inhibitor originally developed by Roche and firs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/12
CPCC07D305/12
Inventor 许勇煌彭韪王德刚唐彬喜刘德富
Owner ZHUHAI UNITED LAB
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