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Preparation method of agomelatine I crystal forms

A technology of crystal form and crude product, which is applied in the field of preparation of raw materials, can solve the problems of poor reproducibility and achieve the effect of high purity

Active Publication Date: 2014-04-09
CHENGDU XINJIE HIGH TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, repeated experiments have shown that the method has poor reproducibility

Method used

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  • Preparation method of agomelatine I crystal forms
  • Preparation method of agomelatine I crystal forms
  • Preparation method of agomelatine I crystal forms

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Crude agomelatine was prepared according to the literature "Chinese Journal of Pharmaceutical Industry 2008, 39 (3) 161".

[0033] Add 1.15 kg of crude agomelatine to 2.88 kg of N, N-dimethylformamide (DMF) ethanol solution (5% ethanol, percent by mass), and stir at room temperature (0-35°C) until completely dissolved. Then, filter through an organic filter with a pore size of 0.2 μm. During the stirring process, add 28.8 kg of water to the filtrate, and filter after 2 hours of stirring and crystallization; the solid is beaten and filtered with 1.5 kg of water, a total of 3 times. The obtained solid was dried under normal pressure at 40-80°C to obtain about 1.06kg of solid. Yield: 92%, purity 99%.

[0034] The X powder diffraction data are:

[0035]

[0036] After the X powder diffraction data are indexed, the unit cell parameters are as follows:

[0037] Molecular formula: C 15 h 17 NO 2

[0038] Molecular weight: Mr=243.30

[0039] Crystal system: Orthorho...

Embodiment 2

[0049] The crude agomelatine was dissolved in the following mixed solvents with different concentrations, and the solid was precipitated according to the above-mentioned process (the process was the same as that in Example 1), and a crystalline solid of I was obtained.

[0050] 1. Methanol and DMF:

[0051] Methanol concentration

5%

25%

50%

75%

95%

crystal form

Form I

Form I

Form I

Form I

Form I

[0052] 2. Ethanol and DMF

[0053] Concentration of ethanol

5%

25%

50%

75%

95%

crystal form

Form I

Form I

Form I

Form I

Form I

[0054] 3. Isopropanol and DMF

[0055] Concentration of isopropanol

5%

25%

50%

75%

95%

crystal form

Form I

Form I

Form I

Form I

Form I

[0056] 4. Acetone and DMF

[0057] Concentration of acetone

5%

25%

50%

75%

95%

crystal form

...

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Abstract

The invention discloses a preparation method of agomelatine I crystal forms, which comprises the following steps of A. enabling agomelatine coarse products to be dissolved in mixed solvent of water-solubility organic solvent and dimethyl formamide (DMF) to obtain a mixed system, the mass percentage concentration of the water-solubility organic solvent in DMF is 5%-95%, heating the mixed system to enable the agomelatine coarse products to be dissolved, filtering by using an organic system film with the hole diameter smaller than or equal to 0.2mum, and obtaining filter liquor; B. adding water in the filter liquor, dissolving the solid out, and obtaining dissolved-out solid after filtering; C. enabling the solid obtained in the step B to be pulped by using water, and filtering to obtain solid; and D drying the solid obtained in the step C at the temperature of 40-80 DEG C to obtain the agomelatine I crystal forms. Compared with the prior art, the preparation method has the advantages that the agomelatine I crystal forms prepared by the method are good in repeatability, the yield is as high as 92%, and the purity is as high as 99%.

Description

technical field [0001] The present invention relates to the field of preparation methods of raw materials, in particular to a preparation method of agomelatine I crystal form. Background technique [0002] Agomelatine (agomelatine, 1), chemical name N-[2-(7-methoxy-1-naphthyl) ethyl] acetamide, trade name Valdoxan, is a melatonin developed by the French Servier company An agonist that also antagonizes 5HT2C receptors, it is the first melatonin antidepressant that can effectively treat depression, improve sleep parameters and maintain sexual function. [0003] WO2011054917A reports a preparation method of agomelatine I crystal form. In the method, agomelatine is dissolved in a single water-soluble organic solvent, and then the solid is precipitated by adding water, so as to obtain the desired crystal form. However, repeated experiments show that the method has poor reproducibility. The reason is that when the solid dissolves, there will be a small amount of tiny crystal nu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/18C07C231/24
Inventor 叶丁肖宁李有章
Owner CHENGDU XINJIE HIGH TECH DEV CO LTD
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