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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  • 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 quality cannot be accurately controlled, the crystal form and particle size are difficult to take into account, and it is not suitable for large-scale production.

Method used

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  • Crystallization process of dexibuprofen
  • Crystallization process of dexibuprofen

Examples

Experimental program
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Effect test

Embodiment 1

[0047] The crystallization process of the Dexibuprofen of the present embodiment comprises the following steps:

[0048] Step 1: Add 25Kg of crude dextrobuprofen and 75Kg of acetone to the reaction kettle, stir and heat up to 35°C, after the materials are completely dissolved, filter, wash the filter cake with a little acetone, and concentrate the acetone from the filtrate to dryness under reduced pressure to obtain a white solid .

[0049] Step 2, add 2.5Kg of acetone to the white solid of the concentrate, stir and raise the temperature to 50°C, after the material is completely dissolved, control the stirring speed at 60 rpm, and start to cool down slowly, when the internal temperature is 30°C, the material begins to precipitate;

[0050] Step 3, after observing the precipitation of crystalline materials, keep the temperature and stirring speed unchanged for 0.5h, control the vacuum degree to 0.95atm, and slowly distill out acetone;

[0051] Step 4, until the material is all...

Embodiment 2

[0053] The crystallization process of the Dexibuprofen of the present embodiment comprises the following steps:

[0054] Step 1: Add 25Kg of crude product of Dexibuprofen and 75Kg of acetone into the reaction kettle, stir and heat up to 35°C, after the materials are completely dissolved, filter, wash the filter cake with a little acetone, and concentrate the filtrate to dryness under reduced pressure to obtain a white solid.

[0055] Step 2: Add 2.0Kg of acetone to the white solid, stir and raise the temperature to 50°C. After the material is completely dissolved, control the stirring speed to 80 rpm, and start to cool down slowly. When the internal temperature is 36°C, crystals of the material begin to precipitate;

[0056] Step 3: After observing crystal precipitation, keep the temperature and stirring speed unchanged for 0.5h, control the vacuum degree to 0.90 atm, and slowly distill out acetone;

[0057] Step 4, until the material is all converted into white crystals, turn...

Embodiment 3

[0059] The crystallization process of the Dexibuprofen of the present embodiment comprises the following steps:

[0060] Step 1: Add 25Kg of crude product of Dexibuprofen and 75Kg of acetone into the reaction kettle, stir and heat up to 35°C, after the materials are completely dissolved, filter, wash the filter cake with a little acetone, and concentrate the filtrate to dryness under reduced pressure to obtain a white solid.

[0061] Step 2: Add 1.5Kg of acetone to the white solid, stir and heat up to 50°C, after the material is completely dissolved, control the stirring speed to 40 rpm, and start to slowly cool down, when the internal temperature is 43°C, the material begins to precipitate;

[0062] Step 3: After observing crystal precipitation, keep the temperature and stirring speed unchanged for 0.5h, control the vacuum degree to 0.90 atm, and slowly distill out acetone;

[0063] Step 4, until the material is all converted into white crystals, turn on the vacuum, continue ...

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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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