Preparation method of ibuprofen crystal

A crystallization and seed crystal technology, applied in the field of medicine and chemical industry, can solve the problems that centrifugal filtration is not suitable for application in mass production, is not suitable for grain growth and formation, consumes a large amount of warm water, etc. simple method effect

Active Publication Date: 2016-08-17
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complex preparation process, large investment and high operating cost of this patent, centrifugal filtration is not suitable for mass production
[0006] Application number: CN201010235320.7 provides a method for refining ibuprofen for injection, which requires refining oral ibuprofen. This process successfully solves the problem that the content of impurities in ibuprofen injection may introduce unknown side effects. However, there is no explanation on the particle size and particle size, and it needs to consume a large amount of warm water to wash it in the later stage, which is only suitable for refining and removing impurities, not for the growth and formation of grains

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Add 60kg of ibuprofen crude product to 300L of 40% (V / V) ethanol, heat in a water bath, heat up to 50°C, and stir until the crude product is completely dissolved;

[0032] (2) Add 1.8kg of activated carbon, control the water bath at 50°C and stir for 30min, 300r / min;

[0033] (3) suction filtration while hot, the filter cake is cleaned with 90L40% ethanol, and the filtrate is collected;

[0034] (4) The filtrate is cooled and crystallized with ice-brine, and when it is lowered to 20° C., 0.3 kg of seed crystals are dropped inward, and the crystal is grown by stirring, and the rotating speed is 50 r / min;

[0035] (5) After the crystals are precipitated, keep warm at 25° C. and stir for 1 hour;

[0036] (6) Program cooling, control the cooling rate at 1°C / h, drop the temperature to 10°C; then control the cooling rate at 1.5°C / h to cool to 0°C, and then control the cooling rate at 2°C / h to -5°C , filter out the crystals, rinse the filter cake once with 60L of water, ...

Embodiment 2

[0038] (1) Add 60kg of ibuprofen crude product to 180L of 82% (V / V) ethanol, heat in a water bath, heat up to 60°C, and stir until the crude product is completely dissolved;

[0039] (2) Add 2.4kg of activated carbon, control the water bath at 60°C and stir for 40min, 300r / min;

[0040] (3) Suction filtration while hot, clean the filter cake with 80L82% ethanol, collect the filtrate;

[0041] (4) The filtrate is cooled and crystallized with ice salt water, and when it is lowered to 25° C., 0.6 kg of seed crystals are dropped inward, and the crystal is grown by stirring, and the rotating speed is 60 r / min;

[0042] (5) After the crystals are precipitated, keep warm at 25°C and stir for 1.5h;

[0043] (6) Program cooling, control the cooling rate at 1°C / h, drop the temperature to 10°C; then control the cooling rate at 1.5°C / h to cool to 0°C, and then control the cooling rate at 2°C / h to -5°C , filter out the crystals, rinse the filter cake once with 35L of water, and dry to ob...

Embodiment 3

[0045] (1) Add 60kg of ibuprofen crude product to 90L of 75% (V / V) ethanol, heat in a water bath, raise the temperature to 70°C, and stir until the crude product is completely dissolved;

[0046] (2) Add 3kg of activated carbon, control the water bath at 70°C and stir for 45min, 300r / min;

[0047] (3) suction filtration while hot, the filter cake is cleaned with 45L of 75% ethanol, and the filtrate is collected;

[0048] (4) The filtrate is cooled and crystallized with icy salt water, and when it is lowered to 30° C., 1.2 kg of seed crystals are dropped inward, and the crystal is grown by stirring, and the rotating speed is 80 r / min;

[0049] (5) After the crystals are precipitated, keep warm at 25° C. and stir for 2 hours;

[0050] (6) Program cooling, control the cooling rate at 1°C / h, drop the temperature to 10°C; then control the cooling rate at 1.5°C / h to cool to 0°C, and then control the cooling rate at 2°C / h to -5°C , filter out the crystals, rinse the filter cake onc...

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Abstract

The invention belongs to the field of medicine and chemical industry, and in particular relates to a preparation method of ibuprofen crystals. The method comprises the following steps: after completely dissolving the crude product of ibuprofen, adding activated carbon to stir and absorb impurities under heat preservation conditions, cooling the filtrate and adding crystal seed crystallization; out, rinse with an appropriate solvent, and dry to obtain the product. The crystals obtained by the invention have high yield, uniform particle size, average particle size between 350-450 μm, less impurity content and a purity higher than 99.9%.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a preparation method of ibuprofen crystals. Background technique [0002] Ibuprofen, chemical name: 2-(4-isobutylphenyl) propionic acid, is a non-steroidal anti-inflammatory drug, and its anti-inflammatory, analgesic and antipyretic effects are 16-32 times stronger than aspirin. Compared with general anti-inflammatory and analgesic drugs, it has stronger effect and less side effects, no obvious side effects on liver, kidney and hematopoietic system, especially less side effects on gastrointestinal tract, can not tolerate aspirin, propazone, indomethacin and other drugs Patients can take this product. This product is suitable for the treatment of rheumatoid arthritis, rheumatoid arthritis, osteoarthritis, ankylosing spondylitis, neuritis, pharyngitis and bronchitis, etc. Ibuprofen is the only antipyretic drug for children jointly recommended by the World...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/30C07C51/43C07C51/47
CPCC07B2200/13C07C51/43C07C51/47C07C57/30
Inventor 韩新利杜德平张玲宋忠文寇祖星康东伟
Owner SHANDONG XINHUA PHARMA CO LTD
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