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Novel method for synthesizing antineoplastic medicine nedaplatin

An anti-tumor drug, nedaplatin technology, applied in the direction of anti-tumor drugs, drug combinations, chemical instruments and methods, etc., can solve the problems of low production cost, long reaction process, short reaction cycle, etc.

Active Publication Date: 2008-11-12
KUNMING GUIYAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The process is lengthy and complicated, and heavy metal ions Ba are introduced 2+ , adding difficulty to the refinement of the final product
[0013] The above synthetic methods of nedaplatin all have long reaction process and disadvantages such as complicated operation, so it is necessary to develop a method for preparing nedaplatin with short reaction cycle, low production cost and high yield.

Method used

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  • Novel method for synthesizing antineoplastic medicine nedaplatin
  • Novel method for synthesizing antineoplastic medicine nedaplatin
  • Novel method for synthesizing antineoplastic medicine nedaplatin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 Glycolic acid 2.1 grams, sodium hydroxide 1.1 grams, mix and stir after water dissolving, adjust pH value to 7 with glycolic acid or sodium hydroxide, add silver nitrate 4.7 grams, stir to generate white precipitate, filter, wash (water 2 times , absolute ethanol 1 time), 40 ℃ of oven dry, weigh, obtain silver glycolate 4.2 grams, productive rate 83.67%, silver content is 58.64% (theoretical value 59.01%).

[0028] Add 10 grams of iodoplatinum, add an appropriate amount of deionized water (about 300ml), stir evenly and heat up to 60°C, slowly add 4 grams of silver glycolate and 3.1 grams of silver nitrate, stir for 3 hours in the dark, filter out AgI, and heat the filtrate to At 40°C, stir and slowly add sodium hydroxide dropwise to adjust the pH value to 7, avoid light and react for 4 hours, transfer the reaction solution to a rotary evaporator and concentrate under reduced pressure to 1 / 8 of the original volume, solids precipitate out, take cold and filter...

Embodiment 2

[0035] 2.1 grams of glycolic acid, 1.1 grams of sodium hydroxide, mixed and stirred after water-soluble, adjust the pH value to 7 with glycolic acid or sodium hydroxide, add 4.7 grams of silver nitrate, stir to form a white precipitate, filter, wash (water 2 times, anhydrous ethanol 1 time), dried at 40°C, and weighed to obtain 4.1 grams of silver glycolate, with a yield of 81.09% and a silver content of 58.75%.

[0036] Add 10 grams of iodoplatinum, add an appropriate amount of deionized water (about 300ml), stir evenly and heat up to 60°C, slowly add 4 grams of silver glycolate and 3.2 grams of silver nitrate, stir for 3 hours in the dark, filter out AgI, wash with AgI for 2 Once, combine the filtrate and washing water, about 430ml in total, heat to 40°C, stir and slowly add sodium hydroxide dropwise to adjust the pH value to 7, keep away from light and react for 4 hours, transfer the reaction solution to a rotary evaporator and concentrate under reduced pressure After reach...

Embodiment 3

[0043] 2.1 grams of glycolic acid, 1.1 grams of sodium hydroxide, mixed and stirred after water-soluble, adjust the pH value to 7 with glycolic acid or sodium hydroxide, add 4.7 grams of silver nitrate, stir to form a white precipitate, filter, wash (water 2 times, anhydrous ethanol 1 time), dried at 40°C, and weighed to obtain 4.2 grams of silver glycolate, with a yield of 83.06% and a silver content of 58.82%.

[0044] Add 10 grams of iodoplatinum, add an appropriate amount of deionized water (about 300ml), stir evenly and heat up to 60°C, slowly add 4 grams of silver glycolate and 3.2 grams of silver nitrate, stir for 3 hours in the dark, filter out AgI, wash with AgI for 2 Once, combine the filtrate and washing water, about 420ml in total, heat to 40°C, stir and slowly add sodium hydroxide dropwise to adjust the pH value to 7, keep away from light and react for 4 hours, transfer the reaction solution to a rotary evaporator and concentrate under reduced pressure After reachin...

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Abstract

The invention discloses a method for making antineoplastic medicine nedaplatin C2H8N2O3Pt. The method comprises the following technological processes that: cis-diiododiaminoplatinum (II) is taken as reactant; an amount of water is added in the reactant and is evenly stirred; then, argentum glycolate C2H3O3Ag and AgNO3 are slowly added in the solution with the molar ratio Pt (NH3) 2I2: C2H3O3Ag:AgNO3 equal to 1:1:1, and are reacted at a temperature of between 50 and 60 DEG C for 2 to 3 hours; after solid is filtered out, the filtrate is heated to 40 DEG C, and the pH value of the filtrate is adjusted to 7 by NaOH; the obtained solution is heated to 50 to 60 DEG C so as to carry out reaction for 4 hours; finally, the reaction liquid undergoes decompression condensation to obtain nedaplatin solid. The method has short process flow, high yield (above 56 percent) and high product purity.

Description

technical field [0001] The invention relates to platinum antitumor drugs, in particular to the preparation of platinum antitumor drug nedaplatin. Background technique [0002] Nedaplatin (254-S) is the third-generation platinum-based antineoplastic drug after cisplatin and carboplatin. Its English name is Nedaplatin, and its chemical name is cis-glycolic acid-diammineplatinum (II) II)], molecular weight is 303.20, chemical structural formula: [0003] [0004] Nedaplatin was developed by Shionogi Company in Japan and was approved for marketing in Japan in June 1995. At present, this variety has been localized by Nanjing Dongjie Pharmaceutical Co., Ltd., and the product name is Jiebaishu. Nedaplatin is characterized by good water solubility (14.3g / l); small toxic and side effects, dose-limiting toxicity is bone marrow suppression, no nephrotoxicity and neurotoxicity; wide anti-cancer spectrum, effective for head and neck cancer, ovarian cancer, esophageal cancer, Bladder...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00A61P35/00
Inventor 丛艳伟普绍平朱泽兵王庆琨刘祝东高传柱
Owner KUNMING GUIYAN PHARMA
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