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Preparation method for adefovir dipivoxil ester waterless crystallization article, prepared adefovir dipivoxil ester waterless crystallization article and uses thereof

A technique for adefovir dipivoxil and anhydrous crystallization, which is applied in the field of preparation of adefovir dipivoxil anhydrous crystallization, and can solve problems such as general crystallization yield and crystallization purity

Active Publication Date: 2009-01-14
STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystallization yield and crystallization purity of the preparation method of the adefovir dipivoxil anhydrous crystal disclosed in the invention are generally

Method used

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  • Preparation method for adefovir dipivoxil ester waterless crystallization article, prepared adefovir dipivoxil ester waterless crystallization article and uses thereof
  • Preparation method for adefovir dipivoxil ester waterless crystallization article, prepared adefovir dipivoxil ester waterless crystallization article and uses thereof
  • Preparation method for adefovir dipivoxil ester waterless crystallization article, prepared adefovir dipivoxil ester waterless crystallization article and uses thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Dissolve 100g of crude adefovir dipivoxil in 200ml of 95% ethanol, heat to 40°C to dissolve, then cool to 10°C, and put it into a constant pressure funnel. Add 3000ml of isopropyl ether into a 5000ml three-necked flask, stir and cool to 2°C, and then add the adefovir dipivoxil solution to the isopropyl ether dropwise. Then it was kept at 2°C and stirred for 25 minutes, filtered, the filter cake was washed with isopropyl ether, and dried under reduced pressure at 50°C to obtain 96.5 g of adefovir dipivoxil as anhydrous crystals. The content of 99.8% is determined by HPLC. The X-ray powder diffraction spectrum is shown in Figure 1, the infrared absorption spectrum is shown in Figure 2, and the DSC diagram is shown in the attached file. image 3 .

Embodiment 2

[0017] Dissolve 100g of crude adefovir dipivoxil in 200ml of 95% ethanol, heat to 45°C to dissolve, then lower the temperature to 12°C, and put it into a constant pressure funnel. Add 3000ml of n-butyl ether into a 5000ml three-necked flask, stir and cool to 3°C, and then add the adefovir dipivoxil solution to the n-butyl ether dropwise. Then it was kept at 3°C ​​and stirred for 30 minutes, filtered, and the filter cake was washed with n-butyl ether and dried under reduced pressure at 45°C to obtain 98 g of adefovir dipivoxil as anhydrous crystals. The content of 99.6% is determined by HPLC. The X-ray powder diffraction spectrum is shown in Figure 1, the infrared absorption spectrum is shown in Figure 2, and the DSC diagram is shown in the attached file. image 3 .

Embodiment 3

[0019] Dissolve 100g of crude adefovir dipivoxil in 200ml of 95% ethanol, heat to 50°C to dissolve, then lower the temperature to 11°C, and put it into a constant pressure funnel. Add 3000ml of sec-butyl ether into a 5000ml three-necked flask, stir and cool to 4°C, and then add the adefovir dipivoxil solution to the sec-butyl ether dropwise. Then it was kept at 2°C and stirred for 0.5hr, filtered, the filter cake was washed with sec-butyl ether, and dried under reduced pressure at 50°C to obtain 98.3g of adefovir dipivoxil as anhydrous crystals. The content of 99.8% is determined by HPLC. The X-ray powder diffraction spectrum is shown in Figure 1, the infrared absorption spectrum is shown in Figure 2, and the DSC diagram is shown in the attached file. image 3 .

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Abstract

Disclosed is a preparation method of an adefovir dipivoxil anhydrous crystal mass, the acquired adefovir dipivoxil anhydrous crystal mass as well as applications thereof, comprising the steps of: A. dissolving a crude product of adefovir dipivoxil with 95 percent ethanol; B. adding ether into a crystallization kettle, agitating the mixture and cooling the temperature to between 2 and 5 DEG C, adding the dissolved solution of adefovir dipivoxil acquired in the step A into the crystallization kettle, and agitating the mixture until reaching crystallization; and filtering the crystal mass, collecting a wet product of the crystal mass and then drying the wet product, wherein, the ether is one or more of iso-propyl ether, n-butyl ether and sec-butyl ether. The obtained crystallization yield reaches over 96 percent, and the crystal mass purity reaches above 99.5 percent. The adefovir dipivoxil anhydrous crystal mass is applied to the preparation of medicines for curing anti-hepatitis B viruses, and has good product activity.

Description

Technical field [0001] The present invention relates to the field of nucleoside drugs, in particular to a preparation method of adefovir dipivoxil anhydrous crystals, the obtained products and applications thereof. Background technique [0002] Adefovir dipivoxil, its chemical name is: 9-{[2-[[bis(pivaloyloxy)methoxy]phosphoryl]methoxy]ethyl}adenine, a new type of HBV Adefovir dipivoxil, a DNA polymerase inhibitor, can effectively inhibit the replication of HBV DNA and rapidly reduce the HBV DNA titer. In patients with lamivudine resistance, adefovir dipivoxil can continue to effectively inhibit mutant strains. It has shown better effects on human and animal retrovirus infections (such as HIV, SIV, FIV, etc.), various hepatitis virus infections (such as HBV, HCV, etc.), and DNA virus infections (such as herpes virus, HSV1, HSV2, etc.). Good antiviral activity. [0003] The currently disclosed crystals of adefovir dipivoxil have high production costs and low purity of the crystals...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6561A61K31/675A61P1/16A61P31/12
Inventor 龚美义瞿东方鲁立崔锦栋
Owner STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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