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Meloxicam compound and purifying method thereof

A kind of technology of meloxicam and purification method, which is applied in the field of medicine and can solve the problems such as the inability to substantially improve the purity

Inactive Publication Date: 2010-02-03
HAINAN YONGTIAN PHARMA INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN101090900A provides a method for the preparation of high-purity meloxicam, the crude product of meloxicam is reacted with potassium hydroxide or potassium carbonate solution, thereby generating high-purity meloxicam potassium salt monohydrate, followed by inorganic Treat the salt with acid or organic acid to generate high-purity meloxicam. This method does not take purification methods after meloxicam is formed into a salt, and cannot essentially improve its purity.

Method used

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  • Meloxicam compound and purifying method thereof
  • Meloxicam compound and purifying method thereof
  • Meloxicam compound and purifying method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Dissolve 7g of meloxicam crude product (97.7% purity) in 300ml of dichloromethane-methanol (91:9) and add it to the top of the column. Silica gel. The length of the column is 20cm, the diameter is 3cm, the column pressure is 0.1pa, and then pumped into dichloromethane-methanol (91:9) for column chromatography, the flow rate is 0.5cm / min, the column temperature is kept at 30°C, start timing, sampling, and follow-up monitoring , collected in sections, collected the liquid, washed with water, dried over anhydrous sodium sulfate, concentrated under reduced pressure, and evaporated the eluent to obtain 6.5 g of meloxicam purified product, with a yield of 92.8%, a melting point of 247°C, and a purity of 99.9%. .

Embodiment 2

[0026] Dissolve 28g of meloxicam crude product (purity: 97.3%) in 800ml of dichloromethane-methanol (95:5) and add it to the top of the column. Silica gel. The length of the column is 20cm, the diameter is 3cm, the column pressure is 4.0pa, and then pumped into dichloromethane-methanol (95:5) for column chromatography, the flow rate is 1.5cm / min, the column temperature is kept at 40°C, start timing, sampling, and follow-up monitoring , collected in sections, collected the liquid, washed with water, dried over anhydrous magnesium sulfate, concentrated under reduced pressure, and evaporated the eluent to obtain 26.1 g of meloxicam purified product, with a yield of 93.2%, a melting point of 248°C, and a purity of 99.8% .

Embodiment 3

[0028] Dissolve 15g of meloxicam crude product (98.0% purity) in 500ml of dichloromethane-methanol (99.9:0.1) and add it to the top of the column. Silica gel. The length of the column is 20cm, the diameter is 3cm, the column pressure is 1.5pa, and then pumped into dichloromethane-methanol (99.9:0.1) for column chromatography, the flow rate is 1.0cm / min, the column temperature is kept at 35°C, start timing, sampling, and follow-up monitoring , collected in sections, collected the liquid, washed with water, dried over activated alumina, concentrated under reduced pressure, and evaporated the eluent to obtain 13.7 g of purified meloxicam, with a yield of 91.3%, a melting point of 246°C, and a purity of 99.9%.

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Abstract

The invention discloses a meloxicam compound and a purifying method thereof. In the method, a simple silica gel column chromatography method is used, proper stationary phases and mobile phases are adopted, i.e. the silica gel is the stationary phase, a mixed solvent of methylene dichloride and methanol with a certain proportion is used as the mobile phase, the temperature of the column is higher than the room temperature, the meloxicam can be efficiently produced and purified, and the yield and the purity are both high. The method is very effective for obtaining the meloxicam with high purity.

Description

technical field [0001] The invention relates to a compound and a purification method thereof, in particular to a purification method of a meloxicam compound, which belongs to the technical field of medicines. Background technique [0002] Meloxicam, chemical name: 4-hydroxy-2-methyl-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3-carboxamide -1,1-dioxide, molecular formula: C 14 h 13 N 3 o 4 S 2 , molecular weight: 351.42, chemical structural formula: [0003] [0004] This product is an enolic acid non-steroidal anti-inflammatory drug (NSAID), which has strong anti-inflammatory, analgesic and antipyretic effects, can inhibit the synthesis of prostaglandins, and is selective for cyclooxygenase-2 (COX-2) Sexual inhibition, more secure than other NSAIDs. It is clinically applicable to the treatment of rheumatoid arthritis and painful osteoarthritis (arthrosis, degenerative osteoarthritis). [0005] Meloxicam is poorly soluble in water, and has good water solubility ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/12B01D15/08
Inventor 陶灵刚
Owner HAINAN YONGTIAN PHARMA INST