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Method for preparing high purity vincristine sulfate

A vincristine sulfate, high-purity technology, applied in organic chemistry, drug combination, antineoplastic drugs, etc., can solve the problems of unrefined methods and achieve the effect of simple operation

Active Publication Date: 2009-02-11
深圳万乐药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of vincristine obtained by this method is only 80-85%, and there is no further refining method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 2g of vinblastine sulfate was dissolved in 240ml of tetrahydrofuran, and 7.5ml of glacial acetic acid was added. Under its protection, the temperature was cooled to -65°C with dry ice, and under stirring, the prepared sodium dicadmate solution (3g of sodium dicadmate dissolved in 15ml of water, then add 2ml of concentrated sulfuric acid, stir to dissolve), and keep the reaction temperature below -50°C during the dropwise addition. After the dropwise addition was completed, the reaction was stirred at -65°C for 3 hours.

[0021] The reaction solution was poured into a mixed solution of 35ml of concentrated ammonia water and 200ml of water, extracted with 600ml of dichloromethane, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 2.06g of crude vincristine with a purity of 83% by HPLC.

[0022] The obtained vincristine crude product is dissolved in 20ml of isopropanol, under stirring, 16ml of 1% isopropanol solution of sulfuric acid...

Embodiment 2

[0025] 20g of vinblastine sulfate was dissolved in 2400ml of THF, and 75ml of glacial acetic acid was added. Under its protection, the temperature was cooled to -65°C with dry ice, and under stirring, the prepared sodium dicadmate solution (30g of sodium dicadmate dissolved in 1500ml water, then add 20ml of concentrated sulfuric acid, stir to dissolve), and keep the reaction temperature below -50°C during the dropwise addition. After the dropwise addition was completed, the mixture was stirred and reacted at -65°C for 3 hours.

[0026] The reaction solution was poured into a mixed solution of 350ml of concentrated ammonia water and 2000ml of water, extracted with 6000ml of dichloromethane, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 21g of crude vincristine with a purity of 85% by HPLC.

[0027] The obtained vincristine crude product was dissolved with 200ml of isopropanol, under stirring, 160ml of 1% isopropanol solution of sulfur...

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PUM

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Abstract

The invention discloses a preparation method for high-purity vincristine sulfate. The method comprises the following steps: a crude product of the vincristine sulfate dissolves in isopropyl alcohol, is stirred, and is added with isopropanol sulfate solution for regulating a pH value to be less than or equal to 4, then the solution is filtered and dried, thus obtaining the vincristine sulfate which dissolves in ethanol, then the vincristine sulfate is cooled and stirred, and solid is separated out, and is filtered and washed by ethanol, and then is dried. The preparation method has simple and effective operation and is easy for industrialized production.

Description

technical field [0001] The invention relates to a preparation method of high-purity vincristine sulfate. Background technique [0002] Vincristine is a cell cycle-specific drug that mainly acts on the M phase. Vincristine can specifically bind to tubulin, inhibit microtubule polymerization, prevent spindle formation, and terminate cell nuclear division. Its curative effect on animal tumors exceeds that of vinblastine. [0003] Chinese patent application CN1724539A discloses a method for purifying vinblastine and vincristine. The method obtains vincristine by extracting and purifying the crude extract of vinca flower. The disadvantage of this method is that the yield of vincristine is low, only 5.8%, which is unfavorable for the industrialized production of vincristine. European patent application EP0037290 discloses a method for synthesizing vincristine: taking vinblastine sulfate as a raw material and obtaining vincristine through oxidation. The purity of vincristine obta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D519/04A61P35/00
Inventor 苏云淡吴子强张广明
Owner 深圳万乐药业有限公司
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