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Preparation method of beta-crystal form silodosin

A technology of silodosin and beta crystal form, applied in the field of preparation of beta crystal form silodosin, can solve problems such as low yield, loss of silodosin, etc. type single effect

Inactive Publication Date: 2014-08-13
WUHAN SYNCHALLENGE UNIPHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this patented method is that the yield is not high, resulting in a large amount of loss of silodosin

Method used

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  • Preparation method of beta-crystal form silodosin
  • Preparation method of beta-crystal form silodosin
  • Preparation method of beta-crystal form silodosin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 5 g of crude silodosin crystals into 20 ml of 2-methyltetrahydrofuran, heat to about 80° C. under a nitrogen atmosphere and reflux for 30 minutes, then cool down naturally. After reaching room temperature, it was filtered and sucked dry. After vacuum drying at 40°C, 4.7g of off-white solid was obtained, with a yield of 94%, a purity of 99.6%, and a melting point of 105-106°C.

[0021] The obtained crystals were measured by X’Pert PRO X-ray diffractometer of PANalytical B.V. company in the Netherlands, Cu target, tube voltage 40 kV, tube current 40 mA, and its X-ray powder diffraction is shown in the attached figure 1 shown

[0022]

Embodiment 2

[0024] Add 4.5 g of crude silodosin crystals to a mixture of 9 ml ethanol and 27 ml 2-methyltetrahydrofuran, heat to about 70° C. under nitrogen atmosphere and reflux for 30 minutes, then cool down naturally. After reaching room temperature, it was filtered and dried, and dried under vacuum at 40°C to obtain 4.1 g of an off-white solid with a yield of 91%, a purity of 99.76%, and a melting point of 105-106°C.

[0025] The obtained crystals were measured by X’Pert PRO X-ray diffractometer of PANalytical B.V. company in the Netherlands, Cu target, tube voltage 40 kV, tube current 40 mA, and its X-ray powder diffraction is shown in the attached figure 1 shown.

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Abstract

The invention provides a preparation method of beta-crystal form silodosin. The preparation method comprises the following steps: adding silodosin into an organic solvent, heating in nitrogen till the refluxed solution is clear, naturally cooling to crystallize after 30 minutes, filtering to obtain white solid, and drying at about 40 DEG C in vacuum, wherein the X-ray powder diffraction spectrum shows that the crystal form of silodosin is beta, the purity is 99.6-99.7%, and the melting point is 105-106 DEG C. The method can stably prepare the beta-crystal form silodosin, and is high in yield and applicable to industrial production.

Description

technical field [0001] The present invention relates to a kind of silodosin (2,3-dihydro-1-(3-hydroxypropyl)-5-[(2R)-2-[2-[2-(2,2,2-tri Fluoroethoxy) phenoxy] ethylamino] propyl] -1H-indole-7-carboxamide) crystal form β preparation method. Background technique [0002] 2,3-Dihydro-1-(3-hydroxypropyl)-5-[(2R)-2-[[2-[2-(2,2,2-trifluoroethoxy)phenoxy] Ethyl] amino] propyl] -1H-indole-7-carboxamide, whose structural formula is shown in (I), referred to as silodosin, is an α1-adrenergic receptor antagonist developed by Japan Tachibana Pharmaceutical Co., Ltd. agent for the treatment of dysuria associated with benign prostatic hyperplasia. [0003] [0004] (I) [0005] US Patent No. 5,387,603 discloses the structure of silodosin and its use in the treatment of dysuria associated with benign prostatic hyperplasia. International Publication WO2004022538 (its Chinese Patent Application No. CN03824796.8) discloses three crystal forms of silodosin, their preparation methods and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/08
CPCC07D209/08
Inventor 刘志平刘慧刘媛吕飞郑文钺王均震
Owner WUHAN SYNCHALLENGE UNIPHARM INC
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