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Process for refining meloxicam

A meloxicam and process technology, which is applied in the refining process field of meloxicam, can solve the problems of low solubility, hidden danger of production safety, instability, etc., and achieves reduction of DMF content, simplified purification process and good safety. Effect

Inactive Publication Date: 2003-01-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] U.S. Patent (US Pat.) 4,233,299 (1980), discloses a refining method of meloxicam is to use tetrahydrofuran to carry out recrystallization, because the solubility of meloxicam in tetrahydrofuran is not large, this method needs to use a large amount of heavy Crystallization solvent, the ratio of solvent to meloxicam is 50:1 (v / w); in addition, tetrahydrofuran is a flammable and explosive organic solvent, and is unstable in the air, and is easily oxidized to form an extremely explosive Peroxides, which bring hidden dangers to production safety, should be avoided
[0004] Another refining method of meloxicam is to use dimethylformamide (DMF) as a recrystallization solvent (Xu Youjun, Liu Feng, Yang Zhimin, Synthetic Chemistry, 1999, 7: 118), although it can purify meloxicam, However, the residual dimethylformamide content in the finished product is very high, usually higher than 1000ppm, far higher than the allowable range of the Chinese Pharmacopoeia, and it is necessary to try to remove the dimethylformamide in the finished product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Refining meloxicam with alkaline absolute ethanol containing sodium hydroxide, the specific steps are as follows:

[0019] 1. Recrystallization of meloxicam:

[0020] Put 20g of meloxicam primary product and 100mL of DMF in a 250mL round bottom flask, heat until the meloxicam is completely dissolved, decolorize with activated carbon, filter, cool the filtrate until the meloxicam crystals are completely precipitated, filter, collect the solid, Obtain 17g of meloxicam crystals, the recovery rate is not less than 80%;

[0021] 2. Purification of meloxicam:

[0022] Take 10 g of the meloxicam solid obtained in the previous step, dissolve it in 20 mL of alkaline absolute ethanol containing 1.14 g of sodium hydroxide, add dilute hydrochloric acid dropwise under stirring, and its concentration is 6 mol / L until the pH value of the solution is 2 , filtered, and the solid was collected, and washed with ethanol, water, water, and ethanol in turn until neutral to obtain 9.5 grams...

Embodiment 2

[0025] Refining meloxicam with alkaline dehydrated alcohol containing potassium hydroxide, the specific steps are as follows:

[0026] 1. Adopt the method for step 1 among the embodiment 1 to preliminarily purify meloxicam;

[0027] 2. adopt the method for refining meloxicam in step 2 in embodiment 1, and its difference is: just change sodium hydroxide into potassium hydroxide, consumption is 1.59g, the meloxicam finished product that obtains passes through GC-MS According to the test, the residual amount of DMF has dropped from 1200ppm to 8ppm, meeting the requirements of the Chinese Pharmacopoeia.

Embodiment 3

[0029] Refining meloxicam with alkaline propanol containing sodium hydroxide, the specific steps are as follows:

[0030] 1. Take 50 grams of meloxicam primary product and 300 mL of DMF, and use the method of step 1 in Example 1 to preliminarily purify meloxicam to obtain 43 grams of meloxicam crystals;

[0031] 2. The method of step 2 in Example 1 is used to refine meloxicam, the difference is: take 35 g of preliminary purified meloxicam, change absolute ethanol into propanol, and the consumption is 100 mL, and the solution is hydrogenated The sodium content is 5.7g, and dilute hydrochloric acid is added dropwise until the pH value of the solution is 3, and the concentration of dilute hydrochloric acid is 5mol / L to obtain 32.8 grams of meloxicam finished product. After detection by GC-MS, the residual amount of DMF has dropped from 1500ppm to 8ppm. Meet the requirements of the Chinese Pharmacopoeia.

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PUM

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Abstract

A process for refining meloxicam, a new non-steroids antipyretic analgesics, includes such steps as adding the crude meloxicam to dimethyl formamide (DMF), thermal dissolving, decolouring, filtering, cooling the filtrate to educe out crystal; dissolving in alkaline alcohol solution, stirring while dripping the diluted hydrochloric acid to regulate pH value to 2-3, filtering, and washing the collected solid until it become neutral to obtain the product. Its advantages are simple process, no poison, and low DMF content.

Description

technical field [0001] The invention relates to a new non-steroidal antipyretic analgesic, in particular to a refining process of meloxicam. Background technique [0002] Meloxicam is a new non-steroidal antipyretic and analgesic drug, which has high anti-inflammatory activity and particularly good intestinal tolerance, and has no nephrotoxicity. It is effective for rheumatoid arthritis and osteoarthritis Significant curative effect, has been listed in the domestic market in 2001. [0003] U.S. Patent (US Pat.) 4,233,299 (1980), discloses a refining method of meloxicam is to use tetrahydrofuran to carry out recrystallization, because the solubility of meloxicam in tetrahydrofuran is not large, this method needs to use a large amount of heavy Crystallization solvent, the ratio of solvent to meloxicam is 50:1 (v / w); in addition, tetrahydrofuran is a flammable and explosive organic solvent, and is unstable in the air, and is easily oxidized to form an extremely explosive The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D417/12
Inventor 刘学良王俊德于亿年
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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