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Preparation method of agomelatine crystal form I

A technology of agomelatine crystal and agomelatine, which is applied in the field of preparation of agomelatine crystal form I, can solve the problem of low purity, poor reproducibility, and poor reproducibility of agomelatine crystal form I. Insufficient stability and other problems, to achieve the effect of environmental friendliness, low cost and good reproducibility

Active Publication Date: 2018-07-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the disadvantages of agomelatine crystal form I in the prior art, such as low purity, poor reproducibility, and insufficient stability, the present invention provides a high-yield agomelatine that is different from the prior art The preparation method of Ting crystal form I

Method used

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  • Preparation method of agomelatine crystal form I
  • Preparation method of agomelatine crystal form I
  • Preparation method of agomelatine crystal form I

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0019] Example 1 Preparation of agomelatine crystal form I

[0020] In a 10mL reaction flask, weigh 1g agomelatine and 30mg ethyl cellulose and mix them evenly, heat to 130℃ to melt, then add 2mL water, stir at 250rpm at room temperature for 20min, filter, and filter the cake Air-dried at room temperature to obtain 912 mg of a white solid with a yield of 91.2% and a melting point of 99.71°C. The obtained solid was subjected to X-ray powder diffraction and DSC, such as figure 1 with figure 2 As shown, the agomelatine crystal form I obtained in the present invention has the following figure 1 The X-ray powder diffraction pattern shown, and its 2θ and relative intensity are shown in Table 1.

[0021] Table 1 Representation of agomelatine crystal form I 2θ and relative strength

[0022] 2θ / degree

[0023] From figure 1 with figure 2 The results prove that the product is agomelatine crystal form I.

Embodiment 2

[0025] In a 10mL reaction flask, weigh 1g agomelatine and 50mg ethyl cellulose and mix them evenly, heat to 130°C to melt, then add 2mL water, stir at 250rpm for 20min at room temperature, filter, and remove the filter cake. Air-dried at room temperature to obtain 922mg of white solid with a yield of 92.2%. Its PXRD pattern and figure 1 Basically the same, DSC spectrum and figure 2 Basically the same, it is agomelatine crystal form I.

Embodiment 3

[0027] In a 10mL reaction flask, weigh 1g agomelatine and 30mg hypromellose and mix them evenly, heat to 110℃ to melt, then add 2mL water, stir at 150rpm for 15min at room temperature, filter, The filter cake was air-dried at room temperature to obtain 933 mg of a white solid with a yield of 93.3%. Its PXRD pattern and figure 1 Basically the same, DSC spectrum and figure 2 Basically the same, it is agomelatine crystal form I.

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Abstract

The invention discloses a preparation method of an agomelatine crystal form I which is a drug for treating depression. The method comprises the steps as follows: a little EC (ethyl cellulose) or HPMC(hydroxyl propyl methyl cellulose) is added to a crude agomelatine product to be molten at 110-200 DEG C, a heat source is removed, a proper amount of water is added, stirring is performed, filtrationis carried out after crystallization, a filter cake is dried, and the agomelatine crystal form I is obtained. The method is simple and easy to operate, has conditions easy to control, requires no organic solvent and is environmentally friendly, high in yield and suitable for industrial production.

Description

Technical field [0001] The invention belongs to the technical field of medical preparation, relates to the field of preparation of raw materials, and specifically relates to a preparation method of agomelatine crystal form I. Background technique [0002] Agomelatine, the chemical name is N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide, the trade name is Valdoxan, developed by the French Servier company. Agomelatine is melatonin 1, 2 (MT 1 , MT 2 ) Receptor agonist, but also serotonin 2c (5-HT 2C ) Receptor antagonist, clinically used to treat depression, regulate sleep and biological rhythms, its safety and tolerability are better, its adverse reactions are relatively weak, and it is comparable to placebo, and there is no sexual dysfunction and withdrawal reaction. It has very important significance and broad market prospects in the treatment of depression. [0003] Agomelatine Form I has been described in detail by Tinant et al. (Actacryst, 1994, 50, 907-910). At present, the prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/18
CPCC07B2200/13C07C231/24C07C233/18
Inventor 施湘君胡盛福宋胜杰丁泽杰苏为科
Owner ZHEJIANG UNIV OF TECH