Purification method of Picoplatin

A purification method and mediplatin technology, applied in the field of platinum antitumor drugs, can solve the problems of low recrystallization yield and low solubility, and achieve the effects of high purity, mild reaction conditions and high yield

Active Publication Date: 2018-03-09
LUNAN BETTER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent uses a mixed solution of N,N-dimethylformamide and hydrochloric acid to dissolve the crude carboplatinum, which has low solubility and low recrystallization yield, and the purity of the obtained products is all below 99%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Dissolve 5.0 g of crude trimethoprim in 55 ml of ether at 50°C, stir for 0.5h, then add 300ml purified water, cool to about 5°C, continue stirring for 1h, filter with suction, and dry for 14h at 100°C to obtain Solid 4.1g, yield 82%, purity 99.96% (HPLC detection), single impurity is less than 0.1%.

Embodiment 2

[0023] Dissolve 5.0g of crude trimethoprim in 25ml dimethyl sulfoxide at 40℃, stir for 0.5h, then add 550ml purified water, cool to about 5℃, continue stirring for 1h, filter with suction, and dry at 100℃ After 14 hours, 4.2 g of solid was obtained, the yield was 84%, the purity was 99.97% (HPLC detection), and the single impurity was less than 0.1%.

Embodiment 3

[0025] Dissolve 5.0g of crude trimethoprim in 30ml ethyl acetate at 20℃, stir for 0.5h, then add 450ml ethanol, cool to about 5℃, continue stirring for 1h, filter with suction, and dry for 14h at 100℃. The obtained solid is 4.2 g, the yield is 84%, the purity is 99.97% (HPLC detection), and the single impurity is less than 0.1%.

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PUM

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Abstract

The invention discloses a purification method of an anti-tumor drug Picoplatin. The technological process comprises the following steps: dissolving a Picoplatin crude product with an organic solvent at a certain temperature; adding a crystallization solvent into the solution for crystallization at a certain temperature; filtering and drying, so as to obtain a Picoplatin highly-finished product. The purification method of the Picoplatin is simple in operation and comparatively high in yield, the purity of the highly-finished product can reach 99.9% or above, a single impurity can be controlledunder 0.1%, and total impurities can be controlled within 0.2%.

Description

Technical field [0001] The invention relates to platinum anti-tumor drugs, in particular to a purification method of trimethoprim. Background technique [0002] Mepyridine platinum, also known as picoplatin and picoplatin, is chemically named cis-dichloro-ammonia, (2-methylpyridine) platinum (Ⅱ) [cis-amminedichloro(2-methylpyridine)–platinate(Ⅱ)] , Is a new generation of anti-tumor drugs. It was first jointly developed by JohnsonMatthey in the United Kingdom, Anormed in Canada and the Cancer Institute in the United Kingdom. It is a new type of platinum complex with steric hindrance, and it has shown good anti-tumor activity both in vivo and in vitro. [0003] The anti-tumor effect of trimethoprim is similar to that of cisplatin, but it is less toxic; it has no cross-resistance to cisplatin and is effective against multiple cisplatin-resistant cells, which can partially overcome the drug resistance caused by cisplatin; it can be administered intravenously or orally medicine. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
CPCC07F15/0093
Inventor 张贵民王洪刚王亚辉刘统郭小为
Owner LUNAN BETTER PHARMA
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