Novel Xtandi crystal form and preparation method thereof

A technology of enzalutamide and crystal form, applied in the field of medicinal chemistry, can solve the problem of not mentioning the spectral characteristics of B1 crystal form enzalutamide, and achieve the effects of good solubility and stable properties

Inactive Publication Date: 2015-02-18
HANGZHOU XINBOSI BIOMEDICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no literature mentioning B1 crystal form enzalutamide and its preparation method, let alone the spectral characteristics of B1 crystal form enzalutamide

Method used

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  • Novel Xtandi crystal form and preparation method thereof
  • Novel Xtandi crystal form and preparation method thereof
  • Novel Xtandi crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 2.0g of enzalutamide solid, add 6ml of mixed solvent (DMSO:toluene=1:2), heat to 90°C, heat to dissolve, cool to 50°C, dilute with 8ml of isopropyl acetate, dilute the diluted solution with 8ml of saturated saline Wash twice, then dry with anhydrous sodium sulfate and filter. The filtrate is spin-dried at 50°C. The oily matter is slurried with 20ml of isopropanol for 16 hours and then filtered. The filter cake is placed in the air at room temperature for 24 hours and then 60°C. After vacuum drying, 1.91 g of enzalutamide in B1 crystal form was obtained, with a yield of 95.5%.

Embodiment 2

[0028] Take 1.2g of enzalutamide solid, add 6ml of mixed solvent (DMSO:1,4-dioxane=1:2) and heat to 90°C to dissolve, then cool to 60°C, add 4ml of 1,4-dioxane After diluting the hexacyclone with 6ml of ethyl acetate, the diluted solution was washed three times with 6ml of water, then dried over anhydrous sodium sulfate and filtered, the filtrate was spin-dried at 60°C, and the oil was mixed with 6ml of a solvent (isopropanol:DMSO=10:1 ) was heated and dissolved at 75°C, cooled to room temperature, filtered, and the filter cake was air-dried at room temperature for 24 hours and then vacuum-dried at 60°C to obtain 1.02 g of enzalutamide in B1 crystal form, with a yield of 85%.

Embodiment 3

[0030] Take 2.0g of enzalutamide solid, add 10ml of mixed solvent (DMSO: isopropyl acetate = 1:4), heat to 80°C to dissolve, cool to 50°C, dilute with 12ml of isopropyl acetate, wash with 12ml of saline Wash twice, then dry with anhydrous sodium sulfate and filter. The filtrate is spin-dried at 60°C. The oily matter is slurried with 20ml of isopropanol for 16 hours and then filtered. The filter cake is placed in air at room temperature for 24 hours and then 60°C. After vacuum drying, 1.86 g of enzalutamide in crystal form B1 was obtained, with a yield of 93%.

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Abstract

The invention provides a novel Xtandi crystal form shown in a chemical formula (I) and a preparation method thereof, and particularly discloses a B1 crystal form Xtandi and a preparation method thereof. The Xtandi disclosed by the invention has the advantages of steady crystal form and good solubility, and the Xtandi is suitable for medicine development. The preparation method is safe and simple, and is strong in maneuverability.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a new crystal form of enzalutamide and a preparation method thereof. Background technique [0002] Enzalutamide, a new oral androgen receptor inhibitor, first launched in the United States in 2012, is indicated for the treatment of patients with advanced metastatic or recurrent castration-resistant prostate cancer, and have undergone drugs or surgery to reduce testosterone treated patients. Because of its good curative effect, safety and few side effects, it has been widely used in clinic. The chemical name of enzalutamide is 4-[3-(4-cyano-3-trifluoromethylphenyl)-5,5-dimethyl-4-oxo-2-thioimidazolidine-1- Base]-2-fluoro-N-methylbenzamide, the structural formula is as shown in formula (I): [0003] [0004] At present, the published patent document of enzalutamide crystal form is patent WO2014 / 041487, which discloses the A2 crystal form of enzalutamide. However, there is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/86
CPCC07D233/86
Inventor 杜焕达罗瑾叶鑫杰王万青刘艳华
Owner HANGZHOU XINBOSI BIOMEDICAL CO LTD
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