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A kind of crystal form of azilsartan intermediate and preparation method thereof

A kind of technology of intermediate and crystal form, applied in the field of medicine, can solve the problems such as the crystal form and crystal preparation method of intermediate compound I of Azisartan are not found

Active Publication Date: 2016-08-31
枣庄市新星钢结构有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, no report on the crystal form and crystal preparation method of azilsartan intermediate compound I has been found.

Method used

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  • A kind of crystal form of azilsartan intermediate and preparation method thereof
  • A kind of crystal form of azilsartan intermediate and preparation method thereof
  • A kind of crystal form of azilsartan intermediate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation method one of the crystal form of Azilsartan intermediate compound I is as follows:

[0026] In a 100mL round-bottom flask, add 5g Azisartan intermediate compound I, add 60mL absolute ethanol, stir, heat to reflux to dissolve all, after refluxing for 1 hour, stop heating, and cool to room temperature (25℃, the same below ), stirring and crystallization at room temperature for 1 hour, filtering, washing with absolute ethanol, and drying to obtain 4.3 g of a white solid sample with a purity of 99.63% and a melting point of 187-189°C.

[0027] The above white solid was subjected to X-ray powder diffraction, and the data obtained are as follows:

[0028] Table 1 Crystal Form X-ray Powder Diffraction Data Table in Example 1

[0029]

[0030]

[0031] However, in the white solid prepared in this example, no regular crystals that can be tested for X-ray single crystal diffraction were not obtained.

Embodiment 2

[0033] Preparation method 2 of the crystalline form of Azilsartan intermediate compound I is as follows:

[0034] In a 100mL round-bottom flask, add 5g Azisartan intermediate compound I, add 100mL ethyl acetate, stir, heat to reflux to dissolve all, after refluxing for 1 hour, stop heating, naturally cool to room temperature, stir at room temperature to crystallize After 1 hour, it was filtered, washed with ethyl acetate, and dried to obtain 4.4 g of a white solid sample of a new crystal form with a purity of 99.54% and a melting point of 186-188°C.

[0035] The above white solid was subjected to X-ray powder diffraction, and the data obtained are as follows:

[0036] Table 2 Crystalline X-ray powder diffraction data table in Example 2

[0037]

[0038]

[0039] However, in the white solid prepared in this example, no regular crystals that can be tested for X-ray single crystal diffraction were not obtained.

Embodiment 3

[0041] The method for cultivating the crystals of Azilsartan intermediate compound I is as follows:

[0042] In a 50mL beaker, add 50mg of Azisartan intermediate compound I, add 10mL of ethyl acetate, heat to dissolve all Azisartan intermediate compound I, stop heating, cool to room temperature, and then add ethyl acetate to 10 mL , Seal the flask with plastic wrap, leave a small hole to slowly permeate the solvent, place it in a stable environment, and let the crystal grow naturally at 20℃. After 3 days, there will be colorless massive crystals. After the crystal growth is complete , Filtered, washed with ethyl acetate, and dried to obtain 43.5 mg of a new crystal sample with a purity of 99.77% and a melting point of 188-189°C.

[0043] After grinding the above crystals into powder, perform X-ray powder diffraction, and the data obtained are as follows:

[0044] Table 3 X-ray powder diffraction data table of the crystal in Example 3

[0045]

[0046]

[0047] Among the crystals prep...

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Abstract

The invention relates to an azilsartan intermediate compound, in particular to preparation methods of a crystal form and a crystal of azilsartan methyl ester. The crystal adopts a triclinic crystal system, the space group is P1, and the cell parameters and the cell volume are specified in the specification. According to the invention, a relatively simple crystallization method is adopted, single solvent is used for recrystallization, the purity of the obtained intermediate reaches higher than 99%, and on the basis, and a purification process of continuously synthesized azilsartan is simplified greatly.

Description

Technical field [0001] The invention belongs to the field of medicine, and specifically relates to a crystal form of azisartan methyl ester and a method for preparing the crystal. Background technique [0002] Angiotensin II receptor antagonists (ARBs) are the latest internationally recommended antihypertensive drugs. They have strong curative effect, no cough side effects, long action time, good patient tolerance, small applied doses, and high trough-to-peak ratio. [0003] Azilsartan, developed by Takeda Pharmaceutical Company of Japan, is a new generation of selective AT1 subtype angiotensin II receptor antagonist antihypertensive drug, which is combined with angiotensin converting enzyme inhibitor (ACEI) Compared with similar antihypertensive drugs, it has the advantages of smoothly reducing blood pressure and not causing dry cough, and the market prospect is very broad. [0004] The hydrolysis of azisartan methyl ester I to prepare azisartan is one of the most commonly used met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D413/10
CPCC07D413/10
Inventor 李正义刘蓉刘大伟钱纪生陈亮孙小强
Owner 枣庄市新星钢结构有限公司
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