Method for purifying irinotecan hydrochloride

A technology of irinotecan hydrochloride and purification method, which is applied in the field of purification of irinotecan hydrochloride to achieve the effects of simple operation, controllable purification conditions and high purity

Active Publication Date: 2010-03-03
CHONGQING TAIHAO PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the defect that there is still adsorbed water in the irinotecan hydrochloride trihydrate purified by the existing irinotecan hydrochloride purification method, and to provide a new method for the purification of irinotecan hydrochloride

Method used

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  • Method for purifying irinotecan hydrochloride
  • Method for purifying irinotecan hydrochloride
  • Method for purifying irinotecan hydrochloride

Examples

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Comparison scheme
Effect test

Embodiment 1

[0033] Dissolve 30 g of crude irinotecan hydrochloride in 60 ml of methanol, cool to 0°C, add 100 ml of ether, stir well, and then stand at 0°C for crystallization for 48 hours, collect the filter cake after suction filtration, and dry in vacuo to obtain 27.4 g of crude product ;

[0034] 27.4 g of the dried crude product were dissolved in 274 ml of methanol, 137 ml of ethyl acetate and 137 ml of acetonitrile were added, stirred evenly, and the pH value of the feed solution was measured to adjust to pH=2. Stand to crystallize at 0°C for 48 hours, collect the filter cake after suction filtration, and dry in vacuo to obtain 25.2 g of crude product;

[0035] Dissolve 25.2 g of the dried crude product in 252 ml of acetone-water ~ 3:1 mixed solution, stir and dissolve, then stand for crystallization at 0°C for 48 hours, collect the filter cake after suction filtration, and place the filter cake in a vacuum-dried Under reduced pressure and drying in the box, the vacuum degree was c...

Embodiment 2

[0037] Dissolve 30 grams of irinotecan hydrochloride crude product in 100 ml of isopropanol, cool to 10°C, add 150ml of petroleum ether, stir evenly, stand for crystallization at 10°C for 8 hours, collect the filter cake after suction filtration, and vacuum dry to obtain Crude product 27.9 grams;

[0038] 27.9 g of the dried crude product were dissolved in 420 ml of ethanol, 279 ml of methyl formate and 279 ml of acetonitrile were added, stirred evenly, the pH value of the feed solution was measured, and adjusted to pH=2. Stand to crystallize at 8°C for 24 hours, collect the filter cake after suction filtration, and dry in vacuo to obtain 26.3 g of crude product;

[0039] Dissolve 26.3 grams of the dried crude product in 390 ml of acetonitrile-water=3:1 mixed solution, stir evenly, and then stand for crystallization at 8°C for 24 hours, collect the filter cake after suction filtration, and place the filter cake in a vacuum-dried Under reduced pressure and drying in the box, t...

Embodiment 3

[0041] Dissolve 30 grams of crude irinotecan hydrochloride in 100ml of isobutanol, cool to 15°C, add 60ml of isopropyl ether, stir evenly, stand at 8°C for crystallization for 24 hours, collect the filter cake after suction filtration, and vacuum dry , to get 26.8 grams of crude product;

[0042] Dissolve 26.8 grams of dried crude product in 134ml of isopropanol, add 134ml of propyl propionate and 134ml of acetonitrile in turn, stir evenly, measure the pH value of the feed solution, adjust to pH=2 with methanol:hydrochloric acid=1:1 mixed solution . Stand to crystallize at 10°C for 8 hours, collect the filter cake after suction filtration, and dry in vacuo to obtain 25.9 g of crude product;

[0043]Dissolve 25.9 grams of the dried crude product in 130 ml of tetrahydrofuran-water mixed solution with a volume ratio of 3:1. After stirring and dissolving, stand for crystallization at 10° C. for 12 hours, collect the filter cake after suction filtration, and place the filter cake ...

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Abstract

The invention discloses a method for purifying irinotecan hydrochloride. The method performs crystallization and purification through three different crystallization systems, the irinotecan hydrochloride is purified by a low-temperature drying method, the purity of the irinotecan hydrochloride in the purified product is up to 99.9 percent, the total impurity content is not more than 0.1 percent, and adsorbed water is not contained. The purifying method has the advantages of controllable conditions, simple operation, low solvent consumption, recycle of irinotecan hydrochloride in the mother liquor and feasible industrial production.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a method for purifying irinotecan hydrochloride. Background technique [0002] Camptothecin was extracted by Wall et al. from the stem and bark of Campylodontaceae in 1966. It uses DNA topoisomerase-I as a target to inhibit the DNA synthesis of cancer cells and exert its anti-tumor effect. However, due to its poor water solubility and unpredictable severe toxicity, its further application is limited. Due to the progress of molecular biology and the deepening of clinical pharmacology research, the climax of designing camptothecin analogues with high efficiency and good water solubility has been stimulated, and irinotecan hydrochloride is one of these research results. [0003] Irinotecan hydrochloride was developed by Japan, and clinical trials began in 1987. Large-scale phase III clinical trials have shown that it is an effective drug for the treatment of metastatic colorectal cancer, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
Inventor 李靖应振培陈波
Owner CHONGQING TAIHAO PHARM CO LTD
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