New crystal form I of agomelatine sulfate and preparation method thereof

A technology of agomelatine and sulfate, which is applied in the field of pharmaceutical chemical synthesis, can solve problems such as research on the crystal form of complexes, and achieve the effects of good fluidity, high bioavailability, and good dissolution rate

Inactive Publication Date: 2013-02-06
FUJIAN COSUNTER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Chinese patent CN200910046782.1 reports the preparation method of agomelatine hydrogen halide complex, and its stability and water solubility are tested, but the crystal form of the corresponding complex has not been studied

Method used

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  • New crystal form I of agomelatine sulfate and preparation method thereof
  • New crystal form I of agomelatine sulfate and preparation method thereof
  • New crystal form I of agomelatine sulfate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Take 10g of agomelatine sulfate and add it to 100ml of ethanol, heat to 80°C to completely dissolve the agomelatine sulfate, then slowly add it dropwise to 400ml of ethyl acetate at room temperature, precipitate a solid, filter , the solid was washed with a little ethyl acetate, and dried under vacuum at 40°C to obtain 9.83g of solid with a yield of 98.3%, a purity of 99.92%, a melting point of 161-162.5°C, and a dissolution rate of 100.4%. See the attached X-ray powder diffraction pattern. figure 2 .

Embodiment 2

[0082] Take 10g of agomelatine sulfate and add it to 100ml of ethanol, heat to 80°C to completely dissolve agomelatine sulfate, then slowly add it dropwise to 500ml of cyclohexane at room temperature, precipitate a solid, filter , the solid was washed with a little cyclohexane, and dried under vacuum at 40°C to obtain 9.81g of solid with a yield of 98.1%, a purity of 99.91%, a melting point of 161.2-162.7°C, and a dissolution rate of 101.5%. See the attached X-ray powder diffraction pattern. figure 2 .

Embodiment 3

[0084] Take 10g of agomelatine sulfate and add it to 80ml of N,N-dimethylformamide, heat to 100°C to completely dissolve agomelatine sulfate, then slowly add it dropwise to 200ml of N,N-dimethylformamide at room temperature In ethyl acetate, a solid was precipitated, filtered, washed with a little ethyl acetate, and dried under vacuum at 40°C to obtain 9.8g of a solid with a yield of 98.0%, a purity of 99.93%, a melting point of 161.5-163.2°C, and a dissolution rate of 100.9%. Its X-ray powder diffraction pattern sees attached figure 2 .

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Abstract

The invention relates to a new crystal form I of an agomelatine sulfate and a preparation method thereof. The preparation method of the crystal form I comprises the steps of heating and dissolving the agomelatine sulfate in a soluble solvent, slowly dripping into an anti-solvent to precipitate crystals, filtering and vacuum drying to obtain the crystal form I. The soluble solvent can be selected from alcohol and amide, and the anti-solvent can be selected from ester and alkane.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical chemical synthesis, and relates to a new crystal form I of agomelatine sulfate and a preparation method thereof. Background technique [0002] The chemical name of agomelatine is N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide, and its structural formula is shown in the following formula (I). Its trade name is Valdoxan, which is the first melatonin-type antidepressant developed by the French company Servier, and it was launched in Germany and the UK in 2009. [0003] [0004] Agomelatine is not only the first melatonin receptor agonist, but also a 5-hydroxytryptamine 2C (S-HTx) receptor antagonist. A large number of animal experiments and clinical studies have shown that the drug has the effects of antidepressant, anti-anxiety, regulating sleep rhythm and regulating the biological clock. At the same time, it has few adverse reactions, no adverse effects on sexual function, and no drug withdr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/18C07C231/24A61K31/165A61P25/24
Inventor 姚建堤陈首鹤陈仕魁杨喜鸿苏葳
Owner FUJIAN COSUNTER PHARMA
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