Crystal form of Pifuadefuwei

A crystal form and crystallization technology, applied in the field of crystal form of pivo adefovir, which can solve the problems of flammability and high cost

Inactive Publication Date: 2003-02-12
CHIA TAI TIANQING PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In addition, the method for preparing AD crystals provided by patent CN1251592A uses expensive, flammable and harmful organic solvents such as n-butyl ether, isopropyl acetate, etc.

Method used

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  • Crystal form of Pifuadefuwei
  • Crystal form of Pifuadefuwei
  • Crystal form of Pifuadefuwei

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 9-(2-phosphonomethoxyethyl)-adenine purification method:

[0045] In a 100L reaction pot, add 1.0Kg of 9-(2-phosphonomethoxyethyl)-adenine crude product into 50L of water, heat to reflux, after dissolving, keep the temperature, add 100g of activated carbon for decolorization for 10min, filter, Let cool to crystallize, filter, and dry the crystals at 80°C to obtain the pure product.

Embodiment 2

[0047] Preparation of Adefovir Pivovir Form E

[0048] In a 10L reaction pot, suspend 0.5Kg (1.8mol) of purified 9-(2-phosphonomethoxyethyl)-adenine in 5L N,N-dimethylformamide, stir, add 1.044KgN, N-dicyclohexyl-4-morpholine, 100ml of triethylamine and 1.382Kg (9.2mol) chloromethyl pivalate, heated up to 50°C, kept stirring for 3 hours, filtered off the insoluble matter, and the filtrate was vacuum-0.1 Concentrate under reduced pressure at Mpa, and extract the concentrate with toluene (10L×2). Recover toluene under reduced pressure at vacuum degree -0.1Mpa, add 5L of pure water to the remaining oily liquid, stir for 5 hours, a large amount of white solid precipitates, filter it out, dissolve it in 1.5L of anhydrous methanol, add anhydrous Stir 1.0Kg of magnesium sulfate for 2 hours, filter, add 50g of activated carbon to the mother liquor, decolorize at 50°C for 10min, take an external bath at 50°C, evaporate to dryness under reduced pressure to obtain a white solid, and dry...

Embodiment 3

[0050] Preparation of Adefovir Pivovir Form E

[0051] In a 10L reaction pot, suspend 0.5Kg (1.8mol) of purified 9-(2-phosphonomethoxyethyl)-adenine in 5L N,N-dimethylformamide, stir, add 1.044KgN, N-dicyclohexyl-4-morpholine, 100ml of triethylamine and 1.382Kg (9.2mol) of chloromethyl pivalate, heated up to 50°C, kept stirring for 3 hours, filtered off the insoluble matter, and vacuum-0.1Mpa Concentrate under reduced pressure, and extract the concentrate with toluene (10L×2). Recover toluene under reduced pressure at vacuum degree -0.1Mpa, add 0.5L of ethanol to the remaining oily liquid, stir to dissolve the oily matter, then add 4L of water, stir for 5 hours, a large amount of white solid precipitates, filter it out, and dissolve it in In 1.5L of anhydrous methanol, add 1.0Kg of anhydrous magnesium sulfate, dry the water, filter, add 50g of activated carbon to the mother liquor, decolorize at 50°C for 10min, use an external bath at 60°C, evaporate to dryness under reduced ...

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Abstract

A crystal form of Adefovir dipivoxil, 9-[2-[[bis (neovaleroxy) methyl] phosphoroso] methoxy]ethyl] adenine, its application to treating hepatism, such as viral hepatitis, its medical composition, and the process for preparing it are disclosed.

Description

technical field [0001] The present invention relates to crystalline form E of 9-[2-[[bis(pivaloyloxy)methoxy]phosphinyl]methoxy]ethyl]adenine. The general name of 9-[2-[[bis(pivaloyloxy)methoxy]phosphinyl]methoxy]ethyl]adenine is adefovir dipivoxil (AD for short). In addition, the present invention also relates to the application of E-type adefovir in the treatment of liver diseases such as viral hepatitis, the pharmaceutical composition containing E-type adefovir and the preparation of E-type adefovir method. Background technique [0002] In Chinese patent CN1251592A (publication number), record 9-[2-[[bis(pivaloyloxy) methoxy] phosphinyl] methoxy] ethyl] invented by U.S. Gillit Science Co., Ltd. Four crystalline forms of adenine and their salts. Among them, the crystalline "form 1" AD basically does not contain water and other crystallization solvents; the crystalline "form 2" is the dihydrate of AD, which usually does not contain other crystallization solvents except w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K31/675A61P1/16A61P31/12C07F9/6561
Inventor 张喜全张爱明徐健
Owner CHIA TAI TIANQING PHARMA GRP CO LTD
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