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A method for preparing tadala amorphous form a

A technology of tadalafil and amorphous form, which is applied in the field of preparation of tadalafil amorphous form A, can solve the problems that it is difficult to fully reduce the residual acetic acid solvent and the cumbersome processing process, and achieve low residual acetic acid solvent and simplify drying Effect of reduction in process and usage

Active Publication Date: 2016-04-06
ZHEJIANG HUAHAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] From the perspective of environmental protection and economic cost, ketones, esters, and alcohol solvents are ideal solvents for preparing crystal form A, but the volume of the above-mentioned solvents is relatively large with the quality of tadalafil, about 55-200ml / g; The acetic acid solvate of tadalafil (the mass ratio of acetic acid volume to tadalafil is 13ml / g), can obtain crystal form A, but the processing process is cumbersome, and it is difficult to fully reduce the solvent residue of acetic acid

Method used

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  • A method for preparing tadala amorphous form a
  • A method for preparing tadala amorphous form a
  • A method for preparing tadala amorphous form a

Examples

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Effect test

Embodiment 1

[0037] Example 1: Preparation of Tadala Amorphous Form A by Using Methanol / Acetic Acid as Solvent

[0038] In a 100ml round bottom flask, add 1.0g of tadalafil and 45ml of methanol / acetic acid mixed solvent (methanol:acetic acid volume ratio 0.8:1). Heated to 83-85°C to obtain a clear solution of tadalafil, and continued to stir for 30-60 minutes. The solution was naturally cooled to room temperature (25-30°C) for crystallization. The solution was further cooled to -5-0°C and stirred for 30-60 minutes for further crystallization. Filter, wash with a small amount of methanol, and drain the solvent to obtain a wet product of Tadalamorph Amorphous Form A. Dry the wet product of tadala amorphous form A at 50-55° C. to obtain 0.5 g of tadala amorphous form A dry product.

Embodiment 2

[0039] Example 2: Preparation of Tadala Amorphous Form A by Using Methanol / Acetic Acid as Solvent

[0040] In a 100ml round bottom flask, add 1.0g of tadalafil and 27ml of methanol / acetic acid mixed solvent (methanol:acetic acid volume ratio 0.6:1). Heated to 83-85°C to obtain a clear solution of tadalafil, and continued to stir for 30-60 minutes. The solution was naturally cooled to room temperature (25-30°C) for crystallization. The solution was further cooled to -5-0°C and stirred for 30-60 minutes for further crystallization. Filter, wash with a small amount of methanol, and drain the solvent to obtain a wet product of Tadalamorph Amorphous Form A. Dry the wet product of tadala amorphous form A at 50-55° C. to obtain 0.5 g of tadala amorphous form A dry product.

Embodiment 3

[0041] Example 3: Preparation of Tadala Amorphous Form A by Using Methanol / Acetic Acid as Solvent

[0042] In a 100ml round bottom flask, add 1.0g of tadalafil and 17.5ml of methanol / acetic acid mixed solvent (methanol:acetic acid volume ratio 0.4:1). Heated to 83-85°C to obtain a clear solution of tadalafil, and continued to stir for 30-60 minutes. The solution was naturally cooled to room temperature (25-30°C) for crystallization. The solution was further cooled to -5-0°C and stirred for 30-60 minutes for further crystallization. Filter, wash with a small amount of methanol, and drain the solvent to obtain a wet product of Tadalamorph Amorphous Form A. Dry the wet product of tadala amorphous form A at 50-55° C. to obtain 0.5 g of tadala amorphous form A dry product.

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PUM

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Abstract

The invention discloses a method for preparing Tadalafil crystal form A. The method is characterized in that the crystallization solvent is a binary mixed solvent of a C1-C4 alcohol and acetic acid or a ternary mixed solvent of a C1-C4 alcohol, acetic acid and water. The method has the characteristics that: a mixed solvent system is used, thus the dosage of the crystallization solvent can be greatly reduced, the drying process can be simplified and the corrosion of acidic materials to the equipment can be reduced.

Description

technical field [0001] The invention relates to a method for preparing tadalamorph A. Background technique [0002] Tadalafil (trade name Cialis, CAS: 171596-29-5), chemical name: (6R-12aR)-2,3,6,7,12,12a-hexahydro-2-methyl-6-( 3,4-(methylenedioxy)-phenyl)-pyrazino[1,2:1,6]-pyrido[3,4-b]indole-1,4-dione, the structural formula is as follows Shown: [0003] [0004] Tadalafil is a drug developed by Eli Lilly for the treatment of male sexual dysfunction. It is a selective and reversible inhibitor of cyclic guanosine monophosphate (cGMP)-specific phosphodiesterase 5 (PDE5). By inhibiting PDE, tadalafil can promote the release of local nitric oxide (NO), thereby stimulating the synthesis of cyclic guanosine monophosphate (cGMP), which further leads to smooth muscle relaxation and increases blood flow, so as to achieve the purpose of treating male impotence. [0005] CN101115484 mentioned in the background technology that according to the reproduction of the process descri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/14
Inventor 姜桥汪伟
Owner ZHEJIANG HUAHAI PHARMA CO LTD
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