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Process for preparing amorphous adefovir dipivoxil

An adefovir dipivoxil and amorphous technology, which is applied in the field of preparation of amorphous organic compounds, can solve the problems of low product purity, many AD impurities and high cost, and achieves the requirements of high purity, reduced temperature conditions, and reduced production. The effect of energy consumption and manufacturing cost

Inactive Publication Date: 2005-09-21
石家庄凯达生物工程有限公司
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this method is that the preparation process needs to be carried out under ultra-low temperature conditions, which consumes a lot of energy and costs high, and this method uses a freeze-drying method to remove the solvent in AD, so the prepared AD has many impurities and low product purity.

Method used

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  • Process for preparing amorphous adefovir dipivoxil
  • Process for preparing amorphous adefovir dipivoxil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] AD crude product can be purchased from the market, and can also be prepared by the following methods:

[0064] Add 4g (0.05mol) PMEA (Adefovir) 2 In a three-necked round-bottomed flask, add 60ml of dry DMF, N-N' dicyclohexyl-4-morpholine 8.32g (0.029mol) and 11g chloromethyl pivalate in turn, stir for 15min, the mixture becomes homogeneous, and at 60 React at ℃ for 4 hours, heat to 60℃ and stir for 4 hours, cool down to 25℃, add 55ml of isopropyl acetate, stir for 30min, filter with suction, wash the filter cake twice with 5ml of isopropyl acetate, and wash the organic layer twice with 10ml of water , the aqueous layer was back-extracted twice with 5ml isopropyl acetate, combined the organic phases, distilled under reduced pressure to an oily substance, added an equal volume of ethanol to dissolve it, added 5 times the amount of water at 0°C, precipitated crystals, and filtered with suction , a white solid was obtained, and dried under reduced pressure to obtain crude ...

Embodiment 2

[0067] Weigh 50g of the crude AD raw material, fully dissolve it with 100ml of absolute ethanol, put it in the refrigerator at -5°C for 6 hours, then quickly add 800ml of -8°C butyl ether at this low temperature, and shake to form a white precipitate. and a suction filter bottle at a low temperature of -10° C. to obtain a white solid, which was vacuum-dried at room temperature to obtain 44 g of AD mainly in an amorphous form (amorphous form was 90%).

Embodiment 3

[0069] Weigh 50g of the crude AD raw material, fully dissolve it with 100ml of acetone, put it in the refrigerator, and freeze it at -2°C for 5 hours. The funnel and filter flask were filtered at -20°C to obtain a white solid, which was vacuum-dried at room temperature to obtain 45 g of AD (85% in amorphous form) with a purity of 98.6%.

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Abstract

The invention discloses a process for preparing amorphous adefovir dipivoxil which comprises charging adefovir dipivoxil into 1-2 times by weight ratio of organic solvent, dissolving and freezing 4-6 hours at -8- -2 deg. C, charging 6-10 times of refrigeration diverting agent under this temperature condition, filtering at -4~-20 deg. C, and vacuum drying.

Description

[0001] Field [0002] The present invention relates to the preparation method of amorphous organic compound, specifically amorphous 9-[2-[[bis(pivaloyloxy)methoxy]phosphinylmethoxy]ethyl]adenine (A defovir dipivoxil, referred to as AD) preparation method. technical background [0003] The state of compounds can be divided into two types: crystalline form and amorphous form. The characteristic of the crystal form is that the particles inside the crystal are regularly arranged in a certain spatial lattice. The characteristics of the amorphous form are that the particles inside the crystal are arranged irregularly, it has high surface energy, good solubility, and high bioavailability. At present, there are many reports on AD crystals. For example, CN1251592A discloses AD in four crystalline forms (namely, anhydrous form, hydrated form, methanol solvated form, fumarate or complex). CN13996170A also discloses a crystalline form substantially free of water and other solvents. L...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6561
Inventor 蒋晔康丽娟张丽芳
Owner 石家庄凯达生物工程有限公司
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