Method of preparing nedaplatin with ultra-low content of silver

A nedaplatin, extremely low technology, applied in the field of preparation of nedaplatin with extremely low silver content, can solve the problems of unstable product quality, low silver content of nedaplatin, high silver content of nedaplatin, etc. Achieve the effects of easy industrial production, extremely low silver content, and reduced deposition

Active Publication Date: 2007-08-08
NANJING HAIRUN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to overcome the shortcomings of the high silver content of nedaplatin obtained by the above-mentioned preparation method of nedaplatin and the insufficient stab

Method used

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  • Method of preparing nedaplatin with ultra-low content of silver
  • Method of preparing nedaplatin with ultra-low content of silver
  • Method of preparing nedaplatin with ultra-low content of silver

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 9.7g (0.02mol) cis-diiododiammine platinum and 30ml water into the reaction flask, stir and mix well, add 6.8g AgNO 3 (0.04mol) dissolved in 40ml of water, the brown-yellow precipitate in the reaction flask turned into pale yellow precipitate, stirred at 20°C for 5 hours, suction filtered to remove the silver iodide, 0.2g potassium iodide (1.2mmol) was added to the filtrate, 20 The reaction was stirred at °C for 1 hour, filtered through a membrane filter, 2g sodium glycolate (0.02mol) was added to the filtrate, the pH was adjusted to neutral with 2N NaOH solution, the temperature was raised to 60 °C, the reaction was stirred for 10 hours, and concentrated under reduced pressure to precipitate a solid , Filtered and dried to obtain 3.4 g of nedaplatin, yield: 56%.

[0019] Detected by atomic absorption spectrophotometry, the silver content of nedaplatin is less than 3ppm; analyzed by high performance liquid chromatography, the content of nedaplatin is 99.65% and related ...

Embodiment 2

[0022] Prepared according to known technology: add 9.7g (0.02mol) cis-diiododiammine platinum and 30ml water into the reaction flask, stir and mix well, add 6.8g AgNO 3 (0.04mol) dissolved in 40ml of water, the brown-yellow precipitate in the reaction flask turned into a light yellow precipitate, stirred at 20°C for 5 hours, suction filtered to remove the silver iodide, and 2g sodium glycolate (0.02mol) was added to the filtrate The pH was adjusted to neutral with 2N NaOH solution, the temperature was raised to 60° C., the reaction was stirred for 3 hours, and concentrated under reduced pressure to precipitate a solid, which was filtered and dried to obtain 3.1 g of nedaplatin. Yield: 51%.

[0023] Detected by atomic absorption spectrophotometry, the silver content of nedaplatin is 300ppm; analyzed by high performance liquid chromatography, the content of nedaplatin is 98.93% and related substances are 0.99%.

Embodiment 3

[0025] Add 14.5g (0.03mol) cis-diiododiammine platinum and 45ml water to the reaction flask, stir and mix well, add 10.2g AgNO 3 (0.06mol) dissolved in 60ml water, stirred and reacted at 30°C for 5 hours, filtered with suction, 0.5g potassium iodide (3mmol) was added to the filtrate, stirred for 1 hour at 25°C, filtered through a membrane, and 2.9g glycolic acid was added to the filtrate Sodium (0.03mol), adjusted pH to neutral with 2N NaOH solution, heated to 60°C, stirred for 8 hours, concentrated under reduced pressure, and solid precipitated out, filtered and dried to obtain 5.4g of nedaplatin, yield: 59%.

[0026] Detected by atomic absorption spectrophotometry, the silver content of nedaplatin is less than 3ppm; analyzed by high performance liquid chromatography, the content of nedaplatin is 99.69%, and the related substance is 0.33%.

[0027] Elemental analysis of nedaplatin prepared in Example 2 and nedaplatin prepared in Example 3 is consistent with the elemental content ...

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Abstract

The invention discloses a making method of naiad platinum with low-silver content, which comprises the following steps: reacting cis-platinum diiododiamide and silver nitrate with molar rate at 1: 2 for 3-8 h under 10-30 deg.c; filtering; adding halogenate MX [M is Na, K, Ca, Ba, NH4 or M is (CnH2n+1) 4N (n=1-4), X=Cl, Br, I] in the filtrate to remove trace silver; reacting for 0.5-1h under 10-30 deg.c; filtering; adding sodium glycolate in the solution; adjusting pH value to neutral to react for 3-10 h under 50-60 deg.c; decompressing; condensing; filtering; drying; obtaining the product; setting the molar rate of cis-platinum diiododiamide and sodium glycolate at 1: 1 and the molar rate of halogenate MX and silver nitrate at 0.1-0.01:1.

Description

Technical field [0001] The invention relates to a preparation method of nedaplatin with extremely low silver content. Background technique [0002] Nedaplatin is a new generation of platinum complex anti-tumor drug after cisplatin and carboplatin. Its trade name is Aqupla and its synonym: 254-S, NSC-375101D. The chemical name of Nidaplatinum is (Z)-diamine (glycolic acid-O1, -O2,) platinum, and its structural formula is: [0003] [0004] Molecular formula: C 2 H 8 N 2 O 3 Pt, molecular weight: 303.18 [0005] As an anti-tumor drug that came out in the 1970s, cisplatin is recognized as the most important achievement and is now widely used in the treatment of a variety of solid tumors and non-solid tumors. However, cisplatin is prone to drug resistance in clinical applications, and has serious side effects such as nephrotoxicity, which limits its use. Many scholars have successively developed carboplatin and isoproplatin in order to seek different anti-tumor spectrum or anti-tum...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 宗在伟陈祥峰
Owner NANJING HAIRUN PHARM CO LTD
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