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Method for synthesizing dicycloplatin by microwave catalysis

A technology of microwave catalysis and synthesis method, applied in chemical instruments and methods, platinum group organic compounds, platinum group organic compounds, etc., can solve the problems of shortened reaction time, long time, co-precipitation of carboplatin and bicycloplatinum, etc. The effect of short time, simple operation and high product purity

Inactive Publication Date: 2017-08-01
ZHONGQI PHARMA IND HENGSHUN ZHONGQI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the method of CN104693245A, this method has shortened the reaction time to a great extent, but it still appears to be too long, and it is necessary to prevent carboplatin and bicycloplatin from co-precipitation

Method used

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  • Method for synthesizing dicycloplatin by microwave catalysis
  • Method for synthesizing dicycloplatin by microwave catalysis
  • Method for synthesizing dicycloplatin by microwave catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045]Add 1.1994g (3.23mmol) carboplatin and 0.4706g (3.27mmol) 1,1-cyclobutanedicarboxylic acid into 90mL water for injection, react in microwave for 9 minutes, control temperature at 30°C, and then reduce pressure at 35°C Concentrate, and wash the filter cake with ethanol. After vacuum drying, 0.8614 g of bicycloplatinum was obtained, with a yield of 71.8% and a content of 81.0% (HPLC method).

Embodiment 2

[0047] Add 1.2014g (3.24mmol) carboplatin and 0.5374g (3.73mmol) 1,1-cyclobutanedicarboxylic acid into 90mL water for injection, react in microwave for 9 minutes, control temperature at 30°C, and then reduce pressure at 35°C Concentrate, and wash the filter cake with ethanol. After vacuum drying, 0.8871 g of bicycloplatinum was obtained, with a yield of 73.8% and a content of 86.4% (HPLC method).

Embodiment 3

[0049] Add 1.2013g (3.24mmol) carboplatin and 0.6097g (4.23mmol) 1,1-cyclobutanedicarboxylic acid into 90mL water for injection, react in microwave for 9 minutes, control temperature at 30°C, and then reduce pressure at 35°C Concentrate, and wash the filter cake with ethanol. After vacuum drying, 1.0314 g of bicycloplatinum was obtained, with a yield of 85.9% and a content of 96.6% (HPLC method). Gained product proves to be dicycloplatinum (see figure 1 with figure 2 ).

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Abstract

The invention discloses a method for synthesizing dicycloplatin by microwave catalysis. The method comprises the steps: mixing carboplatin and 1,1-cyclobutane dicarboxylic acid in a corresponding ratio as well as a solvent; according to a molar ratio of the carboplatin to the 1,1-cyclobutane dicarboxylic acid of 1:(1 to 1.5), performing a reaction for 9 minutes in microwaves, controlling a temperature of 30 DEG C, then carrying out decompressing condensing at a temperature of 35 DEG C, washing a filter cake with ethyl alcohol, and after vacuum drying, obtaining the dicycloplatin. The method disclosed by the invention has the advantages of convenience for operation, mild reaction condition, short reaction time, high reproducibility ad high product purity.

Description

technical field [0001] The invention belongs to the technical field of drug synthesis, and relates to a new method for preparing anti-tumor derivatives by microwave catalysis. The anti-tumor drug is a bis-dicarboxylic acid diamine complex with platinum, which is named bicycloplatinum. Background technique [0002] Since Barnett Rosenberg discovered the antitumor effect of cisplatin in 1969, cisplatin as an antitumor drug has been widely used in clinical medicine. Although these drugs have therapeutic effects on cancers such as genitourinary cancer, nasopharyngeal cancer, cephalosporin circular carcinoma, and lung cancer, the drugs are toxic and cause serious side effects. Some adverse effects such as nephrotoxicity, neurotoxicity, ototoxicity, nausea and vomiting restrict its dosage and long-term use. Carboplatin, one of the second-generation platinum analog antitumor drugs, has an antitumor range similar to cisplatin and is prone to cross-resistance. The antitumor effect ...

Claims

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Application Information

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IPC IPC(8): C07F15/00A61P35/00
CPCC07F15/0093
Inventor 潘林汪林春周驰刘仁涌
Owner ZHONGQI PHARMA IND HENGSHUN ZHONGQI
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