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Lornoxicam compound and purifying method thereof

A kind of technology of lornoxicam and purification method, which is applied in the field of compound purification and can solve the problems of low purity and the like

Inactive Publication Date: 2011-08-24
HAINAN YONGTIAN PHARMA INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem of low purity of the current lornoxicam compound product, the invention provides a method for purifying the low-purity lornoxicam compound by using silica gel column chromatography separation method

Method used

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  • Lornoxicam compound and purifying method thereof
  • Lornoxicam compound and purifying method thereof
  • Lornoxicam compound and purifying method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 12g of lornoxicam crude product (purity 98.7%) was dissolved in 500ml of isopropanol-acetone (1:1), added to the top of the column, the column was 20cm long, 3cm in diameter, column pressure 0.1pa, then pumped into the isopropanol - Acetone (1: 1) carries out column chromatography, the flow velocity is 1.8cm / min, the column temperature is maintained at 30°C, start timing, sampling, follow-up monitoring, carry out segmental collection, collect the lornoxicam eluate, wash with water, Dry over anhydrous sodium sulfate, concentrate under reduced pressure, and evaporate the solvent to obtain 11.2 g of purified lornoxicam, with a yield of 93.3%, a melting point of 225°C, and a purity of 99.8%.

Embodiment 2

[0032] 42g lornoxicam crude product (purity 98.6%) is dissolved in 800ml isopropanol-acetone (5: 1), adds above column, and column length is 20cm, and diameter is 3cm, and column pressure is 4.0pa, and then pumps into isopropanol - Acetone (5: 1) carries out column chromatography, the flow rate is 0.3cm / min, the column temperature is maintained at 40 ° C, start timing, sampling, follow-up monitoring, carry out segmental collection, collect the lornoxicam eluate, wash with water, Dry over anhydrous magnesium sulfate, concentrate under reduced pressure, and evaporate the solvent to obtain 38.5 g of purified lornoxicam, with a yield of 91.6%, a melting point of 226°C, and a purity of 99.9%.

Embodiment 3

[0036] 30g lornoxicam crude product (purity 98.3%) is dissolved in 600ml isopropanol-acetone (3: 1), add above column, column length 20cm, diameter 3cm, column pressure 2.0pa, pump into isopropanol again - Acetone (3: 1) carries out column chromatography, the flow rate is 1.1cm / min, the column temperature is maintained at 35°C, start timing, sampling, follow-up monitoring, carry out segmental collection, collect the lornoxicam eluate, wash with water, Activated alumina was dried, concentrated under reduced pressure, and the solvent was evaporated to obtain 28.3 g of purified lornoxicam, with a yield of 94.3%, a melting point of 225°C, and a purity of 99.9%.

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Abstract

The invention discloses a lornoxicam compound and a purifying method thereof. In the method, a simple silicagel column chromatography method is used, and a proper stationary phase and a proper mobile phase are used, i.e. silicagel is used as the stationary phase and a mixed solvent of isopropanol and acetone with a certain proportion is used as the mobile phase, the temperature of the column is kept to be higher than the room temperature, and the lornoxicam can be efficiently purified. The method can achieve high yield and high purity, thereby being an effective method for obtaining the lornoxicam with high purity.

Description

technical field [0001] The invention relates to a method for purifying a compound, in particular to a method for purifying a lornoxicam compound, and belongs to the technical field of medicines. Background technique [0002] Lornoxicam (Lornoxicam), the chemical name is 6-chloro-4-hydroxy-2-methyl-N-2-pyridyl-2H-thiophene-[2,3-e]-1,2-thiazine- 3-carbon oxalylethylenediamine-1,1-dioxide, molecular formula: C 13 h 10 ClN 3 o 4 S 2 , molecular weight: 371.82, chemical structural formula: [0003] [0004] Lornoxicam belongs to the non-steroidal anti-inflammatory analgesics, which is a thiazide derivative and has strong analgesic and anti-inflammatory effects. Its mechanism of action includes: 1) inhibiting the synthesis of prostaglandins by inhibiting the activity of cyclooxygenase (COX); but lornoxicam does not inhibit the activity of 5-lipid oxidase, so it does not inhibit the synthesis of leukotrienes, It also does not shunt arachidonic acid to the 5-lipid oxidase ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D513/04B01D15/08
Inventor 陶灵刚
Owner HAINAN YONGTIAN PHARMA INST
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