Method for preparing docetaxel anhydrous crystal

A docetaxel, anhydrous crystallization technology, applied in the direction of organic chemistry, etc., can solve the problems of difficult to control water, easy loss of crystal water, difficult to control product quality, etc., and achieve the effect of good stability

Active Publication Date: 2011-09-14
JIANGSU HENGRUI MEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN1151741A discloses a method for preparing docetaxel trihydrate with a mixed solvent of ethanol and water. The method needs to be carried out under the condition that the relative humidity is controlled at 80% during drying, otherwise the crystal water is easily lost and becomes a non-trihydrate , not easy to control product quality
[0005] CN1548426A discloses the method for preparing docetaxel trihydrate with the mixed solvent of acetone and water, and this method is different because of the drying degree of suction filtration sample, uses P 2 o 5 After vacuum drying, the moisture content is difficult to control within the moisture requirement of trihydrate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The preparation of embodiment 1 docetaxel anhydrous crystals

[0014] Add 15g of docetaxel to 35ml of ethanol, stir in a water bath at 40°C to dissolve, gradually add 35ml of diethyl ether dropwise, if there is turbidity during the dropwise addition, it is necessary to dissolve the turbidity before continuing the dropwise addition, and stir for 2 hours after the dropwise addition is completed. It was then cooled to 25°C and stirred overnight. The precipitated crystals were collected by filtration. Wash the crystals with 25ml of a mixed solution of ethanol / ether = 1:1, and then under a pressure of 0.095MPa, 30°C, P 2 o 5 Dry in the presence of 24 hours to get 13.5g (90%) white crystals, melting point: 182.5-184.5 ° C, optical rotation [α] D27 = -44.8 ° (C 0.55, C 2 h 2 OH).

[0015] The obtained crystals were analyzed by GC, and the residual solvent in the sample was in line with the 2005 edition of the Chinese Pharmacopoeia standard.

Embodiment 2

[0016] The preparation of embodiment 2 docetaxel anhydrous crystals

[0017] 15 g of docetaxel was added to 30 ml of acetone, and stirred in a water bath at 40° C. to dissolve it. After dissolving, gradually add about 30ml of diethyl ether dropwise. If there is turbidity during the dropwise addition, dissolve the turbidity and continue the dropwise addition. After the dropwise addition, stir for 2 hours, then cool it to 25°C and stir overnight. The precipitated crystals were collected by filtration. The crystals were washed with 25 ml of acetone / ether = 1:1 mixed solution. Then under the pressure of 0.095MPa, 30℃, P 2 o 5 Dry in the presence of 24 hours to obtain 14g (93.3%) white crystals, melting point: 182.0-184.0 ° C, optical rotation [α] D27 = -44.5 ° (C 0.55, C 2 h 2 OH).

[0018] The obtained crystals were analyzed by GC, and the residual solvent in the sample was in line with the 2005 edition of the Chinese Pharmacopoeia standard.

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Abstract

The invention provides a method for preparing (2R, 3S)-3-boc amino group-2-oxhydryl-3-phenylpropionic acid-4-carbethoxy-2Alpha-benzoyloxy-5Beta and 20-epoxide-1, 7Beta, 10Beta-trihydroxy-9-oxygen-taxus-11-alkene-13Alpha-ester (docetaxel) anhydrous crystallaria. The method uses mixed organic solvent composed of ethanol / aether or the mixed organic solvent composed of acetone / aether for recrystallization. The method has the characteristics of high yield, good product stability, easy drying and large scale production, etc.

Description

technical field [0001] The invention relates to a preparation method of docetaxel, in particular to a preparation method of docetaxel anhydrous crystals. Background technique [0002] The chemical name of Docetaxel is: (2R,3S)-3-tert-butoxycarbonylamino-2-hydroxy-3-phenylpropanoic acid-4-acetoxy-2α-benzoyloxy-5β , 20-epoxy-1,7β,10β-trihydroxy-9-oxo-taxane-11-ene-13α-ester, a second-generation taxane anticancer drug, can promote tubulin assembly into microtubule tube and inhibit its depolymerization, showing unique anticancer activity. [0003] Those skilled in the art can easily prepare docetaxel according to the technical contents disclosed in CN1931849A. [0004] CN1151741A discloses a method for preparing docetaxel trihydrate with a mixed solvent of ethanol and water. The method needs to be carried out under the condition that the relative humidity is controlled at 80% during drying, otherwise the crystal water is easily lost and becomes a non-trihydrate , not easy to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/14
Inventor 孙飘扬欧加保陈永江
Owner JIANGSU HENGRUI MEDICINE CO LTD
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