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Adefovir dipivoxil anhydrous crystal, preparation method and medicine composition thereof

An adefovir dipivoxil and anhydrous crystallization technology, applied in the field of nucleoside drugs, can solve the problems of high preparation cost and high solvent residue, and achieve the effects of simple preparation method, good fluidity and low cost

Active Publication Date: 2007-10-17
SHANGHAI SHYNDEC PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation cost of this crystalline state is relatively high, and due to the use of solvents with higher boiling points, the solvent residue is higher

Method used

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  • Adefovir dipivoxil anhydrous crystal, preparation method and medicine composition thereof
  • Adefovir dipivoxil anhydrous crystal, preparation method and medicine composition thereof
  • Adefovir dipivoxil anhydrous crystal, preparation method and medicine composition thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Dissolve 100g of adefovir dipivoxil crude product in 1500ml of isopropanol aqueous solution (isopropanol: water = 1:3), heat to 70°C, dissolve, add 5g of activated carbon, filter, and cool the filtrate to 0°C, stirring and crystallizing After 5 hours, filter and air-dry at about 50°C to obtain 95 g of the product. As determined by HPLC, the content is 99.5%. Its X-ray powder diffraction spectrum is shown in Figure 1, its infrared absorption spectrum is shown in Figure 2, and its DSC is shown in Figure 3.

Embodiment 2

[0034] Dissolve 100g of adefovir dipivoxil crude product in 1500ml of acetone aqueous solution, (acetone: water = 1:5), heat to 60°C, dissolve, add 5g of activated carbon, stir for 20 minutes, filter, the filtrate is cooled to 0°C, stir and crystallize After 5 hours, filter and air-dry at about 30°C to obtain 91 g of the product. As determined by HPLC, the content is 99.5%. Its X-ray powder diffraction spectrum is as in Example 1, and its infrared absorption spectrum is as in Example 1.

Embodiment 3

[0036] Dissolve 100g of adefovir dipivoxil crude product in 1500ml of acetonitrile aqueous solution (acetonitrile: water = 1: 4), heat to 70°C, dissolve, add 5g of activated carbon, stir for 20 minutes, filter, the filtrate is cooled to 0°C, stir and crystallize After 5 hours, filter and air-dry at about 60°C to obtain 92g of the product. Its X-ray powder diffraction spectrum is as in Example 1, and its infrared absorption spectrum is as in Example 1.

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Abstract

The invention relates to adefovir dipivoxil anhydrous crystallisate. It is characterized in that : XRD: radiating with Cu-k alpha , x ray powder diffraction spectrum expressed in 2 theta having characteristic absorption peak at 3.2,6.5,8.6, 15.7,19.6,21.6, DSC: DSC converting due to absorbing heat at 80 degree; infrared absorption spectrum : KBr pellet , characteristic absorption peak being at 3287cm-1,3175cm-1,1753cm-1,1254cm-1,1147 cm-1,1025cm-1,970cm-1. The present invention also discloses adefovir dipivoxil anhydrous crystallisate preparation method and its pharmaceutical composition. The inventive adefovir dipivoxil anhydrous crystallisate dissolves quicker than 102 degree crystal form, is high in dissolution, and is stable relative to 94 degree crystal form and not easy to be hygroscopic.

Description

technical field [0001] The invention relates to the field of nucleoside drugs, in particular to anhydrous crystals of adefovir dipivoxil, its preparation method and pharmaceutical composition. Background technique [0002] Adefovir dipivoxil (adegovir dipivoxil) is a new type of HBV DNA polymerase inhibitor, is a new type of antiviral drug, its chemical name is: 9-{[2-(dipivaloyloxymethyl)phosphorus Acylmethoxy] ethyl} adenine, its retrovirus infection (such as HIV, SIV, FIV, etc.), various hepatitis virus infections (such as HBV, HCV, etc.) and DNA virus infection (such as herpes virus, HSV1, HSV2, etc.) showed better antiviral activity. Many patents and documents disclose the relevant information of adefovir dipivoxil, such as: U.S. Patent U.S 4724233; European Patent E.P481214; Starrett et al., Antiviral Res. (1992) 19: 267~273, and J.Med.Chem. (1994) 37: 1857-1864; Benzaria et al., J. Med. Chem. (1996) 39: 4958-4965; Zhang Yong et al., Journal of Shenyang Pharmaceutica...

Claims

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Application Information

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IPC IPC(8): C07F9/6561A61K31/675A61P31/12
Inventor 王国平何康勇赵惠清侯建饶品昌
Owner SHANGHAI SHYNDEC PHARMA CO LTD
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