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: 2009-06-17
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 stability of product quality, and provide a method for preparing nedaplatin with an extremely low silver content, Nedaplatin prepared by the present invention has extremely low silver content and stable quality

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
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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) is dissolved in the solution in 40ml water, and the brownish-yellow precipitation in the reaction bottle turns into light yellow precipitation, 20 ℃ of stirring reaction 5 hours, suction filtration removes the silver iodide that generates, adds 0.2g potassium iodide (1.2mmol) in the filtrate, 20 Stir and react at ℃ for 1 hour, filter with membrane, add 2g sodium glycolate (0.02mol) to the filtrate, adjust the pH to neutral with 2N NaOH solution, raise the temperature to 60℃, stir and react for 10 hours, concentrate under reduced pressure, and precipitate a solid , filtered and dried to obtain 3.4 g of nedaplatin, yield: 56%.

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

Embodiment 2

[0022] Preparation according to known technology: add 9.7g (0.02mol) cis-diiododiammine platinum and 30ml water to the reaction bottle, stir and mix well, add 6.8g AgNO 3 (0.04mol) is dissolved in the solution in 40ml water, and the brownish-yellow precipitate in the reaction bottle turns into light yellow precipitate, 20 ℃ of stirring reaction 5 hours, removes the silver iodide that generates by suction filtration, adds 2g sodium glycolate (0.02mol) in 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, concentrated under reduced pressure, a solid was precipitated, filtered and dried to obtain 3.1 g of nedaplatinum, yield: 51%.

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

Embodiment 3

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

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

[0027] The nedaplatin obtained in Example 2 and the nedaplatin obtained i...

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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 (nedaplatin), following cisplatin and carboplatin, is a new generation of platinum complex antineoplastic drugs, trade name Aqupla, synonym: 254-S, NSC-375101D. The chemical name of nedaplatin 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] Cisplatin, as an antineoplastic drug that came out in the 1970s, is recognized as the most important achievement, and has been widely used in the treatment of various solid tumors and non-solid tumors. However, cisplatin is prone to drug resistance in clinical application, and has serious side effects such as nephrotoxicity, which limits its use. The effect is stronger, and there is no cross-resistance or toxicity profile with cisplatin, which is the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00
Inventor 宗在伟陈祥峰
Owner NANJING HAIRUN PHARM CO LTD
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