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Method for preparing crystal form A of blonanserin

A crystal form, ethyl piperazine technology, applied in nervous system diseases, organic chemistry, drug combination and other directions, can solve problems such as high toxicity, and achieve the effect of safe production and preparation process

Inactive Publication Date: 2010-06-23
ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the solvent that adopts in the crystallization method disclosed in this document is chloroform, and the toxicity of chloroform to human body is bigger, and the product of general medicine is required to reach less than 0.03% to the residual amount of chloroform

Method used

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  • Method for preparing crystal form A of blonanserin
  • Method for preparing crystal form A of blonanserin
  • Method for preparing crystal form A of blonanserin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 1g of the crude branserin to 6ml of acetone, heat to reflux to dissolve, then cool to room temperature with stirring, and filter after 2 hours. Dry at 60°C. 0.8 g of a sample of Bronanserin crystal form A was obtained. The melting point is 126~127℃. The total related substances (determined by HPLC) were 0.17%, and the single impurity was 0.07%.

Embodiment 2

[0030] Add 1g of the crude branserin to 20ml of acetone, heat to reflux to dissolve, then cool to room temperature with stirring, and filter after 2 hours. Dry at 60°C. 0.78 g of a sample of bonanserin crystal form A was obtained. The melting point is 126~127℃. The total related substances (determined by HPLC) were 0.14%, and the single impurity was 0.06%.

Embodiment 3

[0032] Add 40g of the crude bulanserin to 350ml of acetone, heat to reflux to dissolve, then cool to room temperature with stirring, and filter after 2 hours. Dry at 60°C. 35 g of a sample of Bronanserin crystal form A was obtained. Melting point 125~126℃. The total related substances (determined by HPLC) were 0.30%, and the single impurity was 0.09%.

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Abstract

The invention provides a method for preparing crystal form A of medicament 2-ethylpiperazine-4-(4-fluorobenzene)-5,6,7,8,9,10-hexahydro cyclooctane pyridine for treating atypical psychosis. The method is characterized by comprising the following steps of: ensuring that the 2-ethylpiperazine-4-(4-fluorobenzene)-5,6,7,8,9,10-hexahydro cyclooctane pyridine is dissolved in acetone, isopropanol or ethyl acetate by heating, and then obtaining the crystal form A through recrystallization. The total relevant material (PHLC determination) of the crystal form A of the 2-ethylpiperazine-4-(4-fluorobenzene)-5,6,7,8,9,10-hexahydro cyclooctane pyridine prepared through the method can reach lower than 0.3 percent, and single impurity is lower than 0.1 percent.

Description

Technical field [0001] The present invention relates to the crystal form A of 2-ethylpiperazine-4-(4-fluorobenzene)-5,6,7,8,9,10-hexahydrocyclooctanopyridine (Blonanserin, Blonaserin) The preparation method. Background technique [0002] The general name of 2-ethylpiperazine-4-(4-fluorobenzene)-5,6,7,8,9,10-hexahydrocyclooctanopyridine with the following structural formula is Blonaserin (Blonanserin), Mainly used for the treatment of atypical psychosis. [0003] [0004] Blonanserin [0005] EP385237 and JP4099768A both reported the synthesis method of bonanserin, but did not describe the problem of crystal form. In the literature Analytical Sciences, 2002, 18: 1289-1290, the single crystal diffraction of bonanserin in chloroform is mentioned, which is also the only report on the crystal form of bonanserin. We prepared the crystal according to the above-mentioned literature method, and the crystal form was proved to be crystal form A by X-ray powder diffraction. However, the sol...

Claims

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Application Information

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IPC IPC(8): C07D221/04A61P25/18
Inventor 王俊芳王小妹王哲烽时惠麟王小梅隋强
Owner ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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