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Method for refining dexrazoxane

A technology of dextropropimine and triethylamine, applied in the field of refining dextropropimine, can solve the problems of high residual solvent, low purity and dark color in the product, and achieve the effects of high purity, good color and high yield

Active Publication Date: 2009-12-02
JIANGSU AOSAIKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the shortcomings of high residual solvent, dark color, low purity and low yield of the product refined by the above-mentioned method for refining dextropropylimine, and to provide a method for refining dextropropylimine, which is an effective A refining method for dextropropanimine that removes the color of the crude product, has high product purity, is simple and convenient to operate, has a short production cycle, high yield, and is easy for industrial production

Method used

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  • Method for refining dexrazoxane
  • Method for refining dexrazoxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 50 g of the crude product of dextropropylimine (content 96.50%, pink), add 200 ml of methanol, add hydrogen chloride methanol solution under stirring, the solid gradually dissolves and clarifies and precipitates off-white crystals, adjust the pH value to 1, filter, discard the filtrate, and Mix the filter cake with 200ml of methanol, adjust the pH value to 8 with triethylamine under stirring, filter, rinse the filter cake with methanol, filter dry, and dry under vacuum at 40°C to obtain 44.5 g of white crystals of dextropropylimine, with a yield of 89.0%; The content detected by HPLC is: 99.92%.

[0021] Determine according to high performance liquid chromatography (two appendix V D of Chinese Pharmacopoeia edition in 2005)

[0022] HPLC chromatographic conditions: octadecylsilane bonded silica gel is used as filler; methanol-0.01mol / L potassium dihydrogen phosphate solution (15:85) is used as mobile phase, and the detection wavelength is 208nm. The number of theo...

Embodiment 2

[0024] Take 20 g of the crude product of dextropropylimine (content 96.50%, pink), add 200 ml of ethanol, add hydrogen chloride ethanol solution under stirring, adjust the pH value to 1, filter, discard the filtrate, mix the filter cake with 200 ml of ethanol, mix with three Adjust the pH value to 8 with ethylamine, filter, rinse the filter cake with ethanol, filter dry, and vacuum-dry at 40°C to obtain 15.5 g of white crystals of dextropropylimine, with a yield of 77.5%; the content detected by HPLC is: 99.63%. HPLC condition is the same as embodiment 1.

Embodiment 3

[0026] Take 10 g of the crude product of dextropropylimine (content 96.50%, pink), add 150 ml of isopropanol, add hydrogen chloride isopropanol solution under stirring, adjust the pH value to 2, filter, discard the filtrate, and mix the filter cake with 200 ml of isopropanol Mix, adjust the pH value to 9 with triethylamine under stirring, filter, rinse the filter cake with isopropanol, filter dry, and vacuum-dry at 40°C to obtain 8.4 g of white crystals of dextropropylimine, with a yield of 84.0%; HPLC detection content For: 99.68%.

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Abstract

The invention relates to a method for refining dextropropyl imine, which comprises mixing and stirring crude dextropropyl imine with 2 to 20 times the amount of C1-3 alkyl alcohol, adding hydrogen chloride or its solution to adjust the pH value to 0.5 to 0.5 5. Filter, mix and stir the filter cake with 2-20 times the amount of C1-3 alkyl alcohol, adjust the pH value to 7-10 with triethylamine, filter, rinse with C1-3 alkyl alcohol, filter dry, 30 Vacuum drying at ~60°C to obtain the refined product of dextropropylimine. The refining method can effectively remove the color of the crude product, has high product purity, is simple and convenient to operate, has short production cycle, high yield and is easy for industrialized production.

Description

technical field [0001] What the present invention relates to is a kind of method of refining dextropropanimine. Background technique [0002] Dexrazoxane, also known as dexrazoxane or ICRF-187, is the dextroisomer of razoxane. The chemical name of dexrazoxane is (s)-(+)-4,4' -(1-methyl-1,2-methylene)-bis(2,6-piperazinedione), its structural formula is: [0003] [0004] Dextropropylimine was developed by Pharmacia & Upjohn Company of the United States. It was approved for marketing in the United States in 1995, and then listed in Canada, France, Italy, Denmark and other countries. It is mainly used as a chemical protective agent in clinical practice, which can effectively prevent anthracycline antineoplastic drugs such Cardiotoxicity induced by doxorubicin, etc., and does not affect the antitumor activity of chemotherapy drugs. It binds to iron ions and interferes with Fe by intracellular hydrolysis into chelating agents 3+ ——The formation of anthracycline chelate, the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/08
Inventor 宗在伟伏世建
Owner JIANGSU AOSAIKANG PHARMA CO LTD
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