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Adefovir dipivoxil CHARIOTEER crystallographic form and preparation method thereof

A technology of adefovir dipivoxil and its crystal form, which is applied in chemical instruments and methods, organic chemistry, and compounds of elements of group 5/15 of the periodic table, etc., can solve the problem of high cost of preparation of adefovir dipivoxil crystal form, lack of Suitable for large-scale industrial production, unfavorable environmental protection and other issues, to achieve good crystal form stability, no reduction in content, and low production costs

Active Publication Date: 2009-07-22
ZHEJIANG CHARIOTEER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Most of the adefovir dipivoxil crystal forms reported in the above literatures have high preparation costs, some solvents are highly toxic, and some methods are not suitable for large-scale industrial production and are not conducive to environmental protection.

Method used

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  • Adefovir dipivoxil CHARIOTEER crystallographic form and preparation method thereof
  • Adefovir dipivoxil CHARIOTEER crystallographic form and preparation method thereof
  • Adefovir dipivoxil CHARIOTEER crystallographic form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Dissolve 45g of adefovir dipivoxil crude product in 150ml of dimethyl carbonate solvent, heat to 40°C, stir to dissolve, filter, cool the filtrate to 10-11°C, crystallize for 5 hours, filter, and obtain solid at 50°C, 5Kpa After vacuum drying for 20 hours, 43.8 g of adefovir dipivoxil crystals were obtained, and the content was 99.6% as determined by HPLC. Cu-Kα radiation, X-ray powder diffraction represented by 2θ angle and interplanar spacing (d value) at about 8.4 (10.8), about 9.8 (9.0), about 14.2 (6.2), about 14.8 (6.0), about 16.2 (5.5), about 17.0(5.2), about 19.7(4.5), about 21.1(4.2), about 22.0(4.1), about 23.1(3.9), about 23.8(3.7), about 25.1(3.6), about 25.6(3.5 ), about 28.8 (3.1), about 29.8 (2.9), about 33.3 (2.6), about 34.6 (2.6), and about 38.9 (2.3) have obvious characteristic absorption peaks, see the attached figure 1 . The differential thermal analysis (DSC) spectrum has an endothermic peak at 94°C, see the attached figure 2 . Infrared absor...

Embodiment 2

[0040] Dissolve 45g of adefovir dipivoxil crude product in 150ml of diethyl carbonate solvent, heat to 40°C, stir to dissolve, filter, cool the filtrate to 14-15°C, crystallize for 5 hours, filter, and obtain solid at 50°C, 5Kpa After vacuum drying for 25 hours, 42.5 g of adefovir dipivoxil crystals were obtained, and the content was 99.7% as determined by HPLC. Cu-Kα radiation, X-ray powder diffraction represented by 2θ angle and interplanar spacing (d value) is at 8.4 (10.9), about 9.8 (9.0), about 14.2 (6.2), about 14.8 (6.0), about 16.2 ( 5.6), about 17.0 (5.2), about 19.7 (4.5), about 21.1 (4.2), about 22.0 (4.1), about 23.1 (3.9), about 23.8 (3.7), about 25.1 (3.6), about 25.6 (3.5) , about 28.8 (3.1), about 29.8 (2.9), about 33.4 (2.6), about 34.6 (2.6), and about 38.9 (2.3) have obvious characteristic absorption peaks. Differential thermal analysis (DSC) spectrum has an endothermic peak at 94°C. Infrared absorption spectrum (KBr tablet) at 3191cm -1 、3122cm -1 、175...

Embodiment 3

[0042] Dissolve 45g of crude adefovir dipivoxil in 150ml of ethyl methyl carbonate solvent, heat to 40°C, stir to dissolve, filter, cool the filtrate to 12-13°C, crystallize for 5 hours, filter, and obtain solid at 50°C, 5Kpa After vacuum drying for 25 hours, 43.2 g of adefovir dipivoxil crystals were obtained, and the content was 99.7% as determined by HPLC. Cu-Kα radiation, X-ray powder diffraction represented by 2θ angle and interplanar spacing (d value) at about 8.4 (10.8), about 9.8 (9.0), about 14.2 (6.3), about 14.8 (6.0), about 16.2 (5.5), about 17.0(5.2), about 19.7(4.5), about 21.1(4.2), about 22.0(4.1), about 23.1(3.9), about 23.8(3.7), about 25.1(3.6), about 25.6(3.5 ), about 28.8 (3.1), about 29.8 (2.9), about 33.3 (2.7), about 34.6 (2.6), and about 38.9 (2.3) have obvious characteristic absorption peaks. Differential thermal analysis (DSC) spectrum has an endothermic peak at 94°C. Infrared absorption spectrum (KBr tablet) at 3189cm -1 、3125cm -1 、1754cm -1 、...

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Abstract

The invention relates to a nucleoside medicinal compound adefovir dipivoxil (abbreviated as "AD", chemical name: 9-[2-[[bis(pivaloyloxy)methoxy]phosphinyl] A new crystal form of methoxy]ethyl)adenine-CHARIOTEER crystal form and preparation method, the CHARIOTEER crystal form uses Cu-Kα radiation, X-ray expressed by 2θ angle and crystal plane spacing (d value) Powder diffraction at about 8.2 (10.9), about 9.8 (9.0), about 14.2 (6.3), about 16.5 (5.5), about 17.0 (5.2), about 19.8 (4.5), about 21.1 (4.2), about 21.5 (4.2) , about 22.5 (3.9), about 23.8 (3.7), about 28.8 (3.1), and about 33.3 (2.6) have characteristic absorption peaks, and the adefovir dipivoxil CHARIOTEER crystal form provided by the present invention has a simple preparation process and is more suitable for industrialization. Production.

Description

(1) Technical field [0001] The present invention relates to a new crystal form of adefovir dipivoxil - CHARIOTEER crystal form, and a preparation method of the new crystal form. (2) Background technology [0002] Adefovir dipivoxil is a nucleoside analogue, a novel HBV-DNA polymerase inhibitor, which can inhibit the activity of hepatitis B virus DNA polymerase, and is a novel anti-hepatitis B virus drug. It has antiviral activity on animals and humans. Therefore, it can inhibit the replication and proliferation of hepatitis B virus. Adefovir dipivoxil has been approved abroad for two indications: patients with chronic hepatitis B and chronic hepatitis B with YMDD mutation resistance after lamivudine treatment. [0003] Adefovir dipivoxil was invented in 1991 by Gilead Sciences Inc. of the United States, applied for a European patent in 1992, and was authorized in 1998. The company did not apply for a patent on the compound in China, but applied for the patent CN1251592A (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6561
Inventor 蒲通雷鸣万定建李东兴王乃星李丰庭范一陈恬
Owner ZHEJIANG CHARIOTEER PHARMA
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