Crystallization process of dexibuprofen

A technology of dexbuprofen and crystallization, which is applied in the field of crystallization technology of dexbuprofen, can solve the problems of inability to accurately control quality, crystal form and particle size, and is not suitable for large-scale production, and achieves that key parameters can be accurately controlled , stable and reliable quality, easy to operate

Active Publication Date: 2021-03-16
湖南华纳大药厂手性药物有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] A crystallization process of Dexibuprofen proposed by the present invention solves the problems in the existing crystallization technology that the qua

Method used

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  • Crystallization process of dexibuprofen
  • Crystallization process of dexibuprofen

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0046] Example 1:

[0047] The crystallization process of the right Blotofen of the present embodiment includes the following steps:

[0048] Step 1. Add 25 kg of ibuprofen crude, 75kg of acetone, stir up to 35 ° C, and the material is fully filtered, filter, filter cake was washed with a small acetone, and the filtrate concentrated to dry, to give a white solid .

[0049] Step 2, 2.5 kg of acetone was added to the concentrate, stirred up to 50 ° C, the material was dissolved, and the stirring speed of 60 rpm was controlled, and the temperature was started slowly, and the temperature was 30 ° C, and the material was precipitated.

[0050] Step three, after the crystal material is precipitated, the temperature is maintained, the stirring speed does not change 0.5 h, control the vacuum 0.95 atm, slowly evaporase the acetone;

[0051] Step four until the material is all converted to a white crystal, turn the vacuum, continuing to evapocetone, and finally transfer the solid to a vacuu...

Example Embodiment

[0052] Example 2:

[0053] The crystallization process of the right Blotofen of the present embodiment includes the following steps:

[0054] Step 1, 25 kg of the right-handed ibuprofen crude, 75 kg of acetone, stirring to 35 ° C, the material was completely filtered, filtered, the filter was washed with a small acetone, and the filtrate was concentrated to dryness to give a white solid.

[0055] Step 2, 2.0 kg of acetone was added to the white solid, stir up to 50 ° C, after the material was dissolved, the stirring speed was 80 rpm, and then slowly cool down. When the temperature was 36 ° C, the material crystal was begun;

[0056] Step three, after crystal precipitation, the temperature is maintained, the stirring speed is not 0.5h, the vacuum is 0.90 atm, and the acetone is slowly evaporated.

[0057] Step four until the material is all converted to a white crystal, turn the vacuum, continuous evaporation, and finally transfer the solid into a vacuum drying tank dry, resulting ...

Example Embodiment

[0058] Example 3:

[0059] The crystallization process of the right Blotofen of the present embodiment includes the following steps:

[0060] Step 1, 25 kg of the right-handed ibuprofen crude, 75 kg of acetone, stirring to 35 ° C, the material was completely filtered, filtered, the filter was washed with a small acetone, and the filtrate was concentrated to dryness to give a white solid.

[0061] Step 2, 1.5 kg of acetone was added to the white solid, stir up to 50 ° C, after the material was dissolved, the stirring speed 40 rpm, the stirring speed was 40 rpm, and the temperature was slowly cooling, and the temperature was 43 ° C, and the material was preciphected;

[0062] Step three, after crystal precipitation, the temperature is maintained, the stirring speed is not 0.5h, the vacuum is 0.90 atm, and the acetone is slowly evaporated.

[0063] Step four until the material is transformed into a white crystal, turn the vacuum, continuing to evapocetone, and finally transfer the so...

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Abstract

The invention discloses a crystallization process of dexibuprofen, which comprises the following steps: step 1, dissolving a dexibuprofen crude product in acetone to obtain an acetone solution, filtering, and concentrating the acetone in filtrate under reduced pressure until the acetone is dry to obtain a solid; step 2, adding acetone into the solid, heating to dissolve, cooling, and stirring to slowly separate out crystals; step 3, after observing that crystals are separated out, keeping the temperature and the rotating speed unchanged, and evaporating out acetone by using micro negative pressure; and step 4, after the material is completely converted into white crystals, starting vacuum to continue to evaporate acetone, and then transferring the solid into a vacuum oven for drying to obtain a finished product. According to the prepared dexibuprofen crystal, the crystal form consistent with that of an original product can be stably obtained, the granularity is uniform, and after crushing, the particle size meeting the requirements of a dexibuprofen preparation can be obtained; the yield can reach 93-98%, the ee% value is greater than or equal to 99.0%, the content of a resolving agent S-phenylethylamine is less than or equal to 0.1%, and the quality is stable and reliable.

Description

technical field [0001] The invention relates to the technical field of medicine purification, in particular to a crystallization process of Dexibuprofen. Background technique [0002] Ibuprofen is a non-steroidal anti-inflammatory analgesic drug, which has stronger antipyretic, anti-inflammatory and analgesic effects than aspirin, and its side effects are much smaller than that of aspirin. It was launched in the UK in 1966 and in 1974. Listed in the United States. In the UK, ibuprofen became the first non-steroidal anti-inflammatory drug that could be sold over-the-counter in 1983; in the second year (1984), ibuprofen also became an over-the-counter drug in the United States. Since its launch, ibuprofen has developed rapidly and has become one of the anti-inflammatory, antipyretic and analgesic drugs with the largest production and usage, with an annual global output of more than 10,000 tons. [0003] [0004] Experiments have proved that dexibuprofen is the active ingr...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C51/43C07C57/30
CPCC07C51/42C07C51/43C07B2200/07C07C57/30
Inventor 罗佳城谭跃蔡国贤谭建国
Owner 湖南华纳大药厂手性药物有限公司
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