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Ibuprofen sodium compound and new preparation method thereof

A technology for ibuprofen sodium and compounds, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., to achieve the effects of compoundability and stability improvement, high product purity, and complete crystal form

Inactive Publication Date: 2013-08-21
HAINAN YONGTIAN PHARMA INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the low defect of existing sodium ibuprofen compound purity, the invention provides a kind of method of refining sodium ibuprofen compound compound

Method used

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  • Ibuprofen sodium compound and new preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 100 ml of 1 mol / L sodium ethoxide to the water phase, stir at 70°C for 2 hours, a solid precipitates, let stand to lower the temperature to room temperature, filter, and collect the filtrate.

[0048] Add the sodium ibuprofen aqueous solution into the crystallization tank, then evacuate the crystallization tank to make the vacuum degree reach -0.10Mpa, then open the hot steam valve on the crystallization tank, and use steam to make the temperature reach 75-80°C for evaporation and concentration;

[0049] Evaporate until the mass percent concentration of ibuprofen sodium in the aqueous solution reaches 55-60%, by closing the heating steam valve, when the temperature is reduced to 55-60°C, close the vacuum valve, open the seeding valve, and prepare in advance A good sodium ibuprofen compound seed crystal is sucked into the crystallization tank, and the seed crystal valve is closed, and then the vacuum valve is opened;

[0050] When it is observed that the sight glass...

Embodiment 2

[0054] Add 200 ml of 1 mol / L sodium methoxide to the water phase, stir at 40°C for 3 hours, a solid precipitates, let stand to lower the temperature to room temperature, filter, and collect the filtrate.

[0055] Add most of the sodium ibuprofen aqueous solution into the crystallization tank, then evacuate the crystallization tank to make the vacuum degree reach -0.15Mpa, then open the hot steam valve on the crystallization tank, and use steam to make the temperature reach 73-78°C for evaporation concentrated;

[0056] Evaporate until the mass percent concentration of ibuprofen sodium in the aqueous solution reaches 53-58%, close the heating steam valve, make the temperature drop to 55-58 °C naturally, close the vacuum valve, open the seeding valve, and the pre-prepared The sodium ibuprofen compound seed crystals are quickly sucked into the crystallization tank, the seeding valve is closed, and then the vacuum valve is opened to complete the seeding work;

[0057] When it is ...

Embodiment 3

[0061] Add 150 ml of 1 mol / L sodium propoxide to the water phase, stir at 50°C for 5 hours, a solid precipitates, let stand to lower the temperature to room temperature, filter, and collect the filtrate.

[0062] Add 60% of the sodium ibuprofen aqueous solution volume in the crystallization tank, then the crystallization tank is vacuumed to a more preferred -0.12Mpa, then by opening the hot steam valve on the crystallization tank, the temperature is reached to 70-75 ° C by steam, carry out evaporation and concentration;

[0063] Evaporate until the mass percent concentration of ibuprofen sodium in the aqueous solution reaches 50-55%, by closing the heating steam valve, the temperature will drop naturally, for example, when it drops to 52-55°C, close the vacuum valve and open the seeding valve , suck the pre-prepared sodium ibuprofen compound seed into the crystallization tank, close the seeding valve, and then open the vacuum valve to complete the seeding work;

[0064] When ...

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Abstract

The invention relates to a method for preparing an ibuprofen sodium compound by the following treatment steps of: 1, dissolving an ibuprofen sodium compound raw material into water, adding a solvent for extracting, separating an organic phase containing impurities, and obtaining an aqueous phase; 2, adding an alkyl oxide of sodium into the aqueous phase for treating, heating in the treatment process, cooling, filtering, and obtaining a filtrate; and 3, performing negative pressure crystallization on the aqueous solution of the ibuprofen sodium, concentrating under negative pressure at a raised temperature, then reducing the temperature, adding ibuprofen sodium compound seed crystal, keeping the temperature when fine crystal grains appear till ideal crystal is obtained, separating, washingand drying the separated crystal, and thus obtaining the refined ibuprofen sodium compound. The ibuprofen sodium compound prepared by the method is uniform in crystal grains, complete in crystal shape, good in flowability and particularly high in treatment quantity, and can be continuously produced, so the method is particularly suitable for industrialized production. Meanwhile, the product quality of the preparation is improved, and the toxic or side effect is reduced.

Description

technical field [0001] The invention relates to a sodium ibuprofen compound and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Sodium ibuprofen, chemical name: 2-(4-isobutylphenyl) sodium propionate dihydrate, molecular formula: C 13 h 18 o 2 Na·2H 2 O, structural formula: [0003] [0004] Sodium ibuprofen is a drug with analgesic, anti-inflammatory and antipyretic properties, which is especially used in the treatment of inflammatory diseases and anti-pain, such as rheumatic diseases, headache, migraine, toothache, back pain, muscle pain, after surgery Pain etc. The analgesic and anti-inflammatory mechanism of this product has not been fully elucidated. It may act on local inflammatory tissues by inhibiting the synthesis of prostaglandins or other transmitters. Due to the inhibition of leukocyte activity and release of lysosomal enzymes, local tissue Pain impulses are reduced and the sensitivity of pain re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/30C07C51/43
Inventor 王明曹丽梅
Owner HAINAN YONGTIAN PHARMA INST
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