A kind of preparation method of rice platinum

A technology of rice platinum and crude products, which is applied in the field of platinum anti-tumor drugs, can solve the problems of low recrystallization yield and low solubility, and achieve the effects of high purity, low production cost and high quality preparations

Active Publication Date: 2017-08-15
SHANDONG LUOXIN PHARMA GRP CO LTD
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But its solubility is small, the recrystallization yield is low, and the product yield obtained is all below 70%.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of rice platinum
  • A kind of preparation method of rice platinum
  • A kind of preparation method of rice platinum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Refinement of Miplatin

[0043] The crude Miplatin used in this example was prepared by the preparation method of Japanese Patent JP11-315088, with a purity of 97.18% (detected by HPLC), a maximum of 1.86% of single impurities, and a total of 3.71% of impurities.

[0044] Refining process:

[0045] 1) Prepare 60 ml of a mixed solution of dimethylformamide and n-butanol (DMF: n-butanol = 2:1), heat up to 145°C, add 5.00 g of Miplatin crude product, keep stirring until completely dissolved, and obtain a Miplatin crude product solution ;

[0046] 2) After the solution is clarified, add activated carbon 0.10g, continue to keep stirring for 30 minutes at a speed of 25 rev / min, filter, and collect the filtrate;

[0047] 3) The filtrate was cooled to 80°C in 1.5 hours, 20ml of toluene was added dropwise in 30 minutes, and then the temperature was kept stirring for 1 hour at a speed of 15 rev / min;

[0048] 4) After the reaction finishes, cool down to 25 ℃ again, s...

Embodiment 2

[0050] Example 2: Refinement of Miplatin

[0051] The crude product of Miplatin used in this example was prepared by the preparation method disclosed in the international patent WO 94 / 14470, with a purity of 95.89% (detected by HPLC), a maximum single impurity of 1.71%, and a total impurity of 3.35%.

[0052] Refining process:

[0053] 1) Prepare 60 ml of a mixed solution of dimethylformamide and n-butanol (DMF: n-butanol = 3:1), heat up to 140 ° C, add 5.00 g of Miplatin crude product, keep stirring until completely dissolved, and obtain a crude Miplatin solution ;

[0054] 2) After the solution is clarified, add activated carbon 0.05g, continue to keep stirring for 40 minutes at a speed of 20 rev / min, filter, and collect the filtrate;

[0055] 3) The filtrate was cooled to 90° C. in 1 hour, and 15ml of toluene was added dropwise in 20 minutes, and then stirred at 10 rev / min for 2 hours;

[0056] 4) After the reaction, the temperature was lowered to 30° C. again, crystals ...

Embodiment 3

[0058] Example 3: Refinement of Miplatin

[0059] The crude Miplatin used in this example was prepared by the preparation method disclosed in European Patent 0193936A1, with a purity of 96.76% (detected by HPLC), a maximum single impurity of 1.58%, and a total impurity of 2.96%.

[0060] Refining process:

[0061] 1) Prepare 50 ml of a mixed solution of dimethylformamide and n-butanol (DMF: n-butanol = 1:1), heat up to 150 ° C, add 5.00 g of Miplatin crude product, keep stirring until completely dissolved, and obtain a crude Miplatin solution ;

[0062] 2) After the solution is clarified, add activated carbon 0.15g, continue to keep stirring for 20 minutes at a speed of 30 rev / min, filter, and collect the filtrate;

[0063] 3) The filtrate was cooled to 70°C within 2 hours, and 25ml of toluene was added dropwise within 40 minutes, and then stirred at 20 rev / min for 0.5 hours;

[0064] 4) After the reaction finishes, cool down to 20 ℃ again, separate out crystals, and grow t...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The present invention provides a preparation method for anti -tumor drugs Miriplatin: prepare a mixed solution for diet metamimam and orthopedly, heating up, add rice platinum coarse products, heat preservation until it is completely dissolved, and the rice platinum coarse solution;After the solution is clarified, add activated carbon to continue the preservation, filter, and collect the filter liquid; cool the filter liquid, add toluene, heat preservation and stir; after the reaction is over, cool down again, precipitate crystals, and keep the crystal.Wash, dry, get Microlatin boutique.The preparation method provided by the present invention is simple, the income is high, the purity of rice platinum reaches more than 99.9 %, the maximum single miscellaneous control is below 0.1 %, and the total miscellaneous control is within 0.2 %.

Description

technical field [0001] The invention relates to platinum antitumor drugs, in particular to a preparation method of meplatin. Background technique [0002] Hepatocellular carcinoma is one of the most common malignant tumors with a high recurrence rate in the world. It ranks fifth in the incidence of malignant tumors and the third in the cause of death in the world. , the number of cases in my country accounts for about 55% of the total number of cases in the world. The pathogenesis of hepatocellular carcinoma is mostly characterized by persistent infection of hepatitis C virus or hepatitis B virus, which leads to chronic hepatitis and liver cirrhosis and eventually develops into hepatocellular carcinoma. Clinically, surgical treatments such as liver resection and transplantation are usually used; local medical treatments such as radiofrequency ablation, percutaneous microwave coagulation therapy, and percutaneous anhydrous ethanol injection therapy; transcatheter hepatic arte...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00
Inventor 高峰李文婷彭红梅
Owner SHANDONG LUOXIN PHARMA GRP CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap