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Crystallization purification method for 10-deacetylbaccatin III

A purification method and deacetylation technology, which is applied in the field of purification of anticancer active ingredients, can solve the problems of low purification efficiency, yield and purity of 10-DABIII, and achieve the effect of simple method, convenient operation and high yield

Inactive Publication Date: 2016-02-24
CHONGQING ZHENYUAN HONGDOUSHAN DEV CO LTD
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AI Technical Summary

Problems solved by technology

At present, the solvent used in the crystallization method in the production process of 10-DABIII is acetone, and the purification efficiency, yield and purity of 10-DABIII after crystallization are relatively low

Method used

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Embodiment

[0017] Weigh 5 groups of 20g 10-DAB crude product with a purity of 35%, add 180ml of acetone to each group, heat to 55°C, and ultrasonically stir at a constant temperature of 55°C for 13min, the 10-DAB crude product is completely dissolved, and the adding temperature is 55°C under ultrasonic stirring 100ml of acetonitrile, stand for crystallization at room temperature for 24 hours, stir evenly, then stand for crystallization in a low-temperature freezer at -25°C for 24 hours, then filter, and dry the wet crystals under hot air at 60°C for 48 hours to finally obtain the product and Determine weight and crystal purity.

[0018] The first group: the product weight is 4.97g, and the purity of 10-DABIII crystal is determined to be 91.46%;

[0019] The second group: the product weight is 5.11g, and the purity of 10-DABIII crystal is determined to be 90.01%;

[0020] The third group: the product weight is 5.01g, and the purity of 10-DABIII crystal is determined to be 91.80%;

[002...

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PUM

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Abstract

A disclosed crystallization purification method for 10-deacetylbaccatin III (10-DAB III) is performed according to the following steps: a, adding acetone into a 10-DAB III crude product, and performing ultrasonic stirring so as to completely dissolve 10-DAB III; b, adding acetonitrile when 10-DAB III is in the state of ultrasonic stirring, and filtering after a crystal is precipitated, so as to obtain a wet crystal; and c, drying the wet crystal, so as to obtain a high-purity 10-DAB III crystal. According to the crystallization purification method for 10-DAB III, by employing the acetone-acetonitrile mixed solvent for crystallization, the purity of the 10-DAB III crude product possessing the purity of 35% and being subjected to once crystallization is improved to 90% or more, the yield is 65% or more, the crystal purity is high, the yield is high, and the method is simple and convenient to operate, and helps to substantially improved the purification yield of 10-DAB III.

Description

technical field [0001] The invention belongs to the technical field of purification of anticancer active ingredients, and in particular relates to a crystallization and purification method of 10-deacetylbaccatin III. Background technique [0002] Paclitaxel is the most active component of the taxane derivatives contained in the southern yew, but as long as it exists in the bark and the content is very small, other components that coexist with it also have certain anticancer activities. And taxol or its analogs can be synthesized through structural modification, in which 10-deacetylbaccatin III (hereinafter referred to as 10-DABIII) is a taxane compound contained in the national first-class protected plant Taxus chinensis, colleagues It is the precursor for the synthesis of paclitaxel and docetaxel. At present, the solvent used in the crystallization method in the production process of 10-DABIII is acetone, and the purification efficiency, yield and purity of 10-DABIII after...

Claims

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Application Information

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IPC IPC(8): C07D305/14
CPCC07D305/14
Inventor 徐道礼徐胜博雷茂林
Owner CHONGQING ZHENYUAN HONGDOUSHAN DEV CO LTD
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