Preparation method of agomelatine I crystal form

A crystal form and crystallization technology, which is applied in the field of medicine, can solve the problems of cumbersome operation and high production cost, and achieve the effects of simple operation, low cost and easy control of reaction conditions

Inactive Publication Date: 2012-08-22
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN200910160307.7 The preparation of V-type agomelatine by spray drying method requires the introduction of inert gas, high production cost and cumbersome operation

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] After heating and melting 50mg agomelatine at 110°C, place the container containing the melted agomelatine in a 20°C water bath and quickly cool it to 20°C, then let it stand, and the obtained crystal form is agomelatine Form I, yield 100%.

Embodiment 2

[0027] After heating and melting 50mg agomelatine at 120°C, place the container containing the melted agomelatine in a 20°C water bath and quickly cool it down to 20°C, then let it stand, and the obtained crystal form is agomelatine Form I, yield 100%.

Embodiment 3

[0029] After heating and melting 50 mg agomelatine at 130°C, place the container containing the melted agomelatine in an ice-water bath to rapidly cool to 4°C, and let it stand still. The obtained crystal form is agomelatine I Crystal form, yield 100%.

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PUM

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Abstract

The invention discloses a preparation method of agomelatine I crystal form. The preparation method comprises the following steps: heating and melting agomelatine at the temperature of 110-200 DEG C, then quickly cooling at the temperature of minus 20-30 DEG C and standing till crystallization. The method used by the invention is simple to operate, reaction conditions are easy to control, the yield is high, any organic solvent is not required, and the obtained crystal form is single, green, environment-friendly and very suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a preparation method of agomelatine I crystal form. Background technique [0002] Agomelatine (Agomelatine), the chemical name is N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide, and its chemical structural formula is as follows (1): [0003] The trade name of agomelatine is Valdoxan, which was first developed by the French company Servier. It is not only the first melatonin receptor agonist, but also a 5-hydroxytryptamine 2C (5HT2c) receptor antagonist, which can effectively treat depression. Anti-anxiety and adjust sleep cycle rhythm. [0004] At present, the method for preparing the crystal form of agomelatine is to first dissolve agomelatine in a solvent, and then extract it. The biggest difference between the current methods is that the solvents used are different. CN101921205A reports a method for preparing agomelatine type I. The drug is heated and dissolved in a mixed s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/18
Inventor 鲁统部耿娜陈嘉媚闫岩
Owner SUN YAT SEN UNIV
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