Preparation method of lobaplatin trihydrate

A technology of lobaplatin trihydrate and aqueous solution, which is applied in the field of preparation of lobaplatin trihydrate, which can solve the problems of no protection measures for acetone, increased requirements for filtration equipment, and increased production costs, so as to reduce impurity intake and shorten concentration Time, time-saving effect

Active Publication Date: 2021-01-15
KUNMING GUIYAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the second method has fewer steps than the first method, but introduces an impurity that is extremely difficult to remove—silver chloride. Although it should be able to be effectively removed by filtering through filter paper and microporous membrane successively, it increases the cost of filtering equipment. Great requirements, but also increased production costs
[0008] In addition, in the above two methods, it takes at least about 20 hours to obtain the product from the recrystallization to the drying stage, and in the recrystallization process, there is no effective protection measure for acetone, a precursor chemical used in large quantities, which is very likely will cause serious production hazards

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  • Preparation method of lobaplatin trihydrate
  • Preparation method of lobaplatin trihydrate
  • Preparation method of lobaplatin trihydrate

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Embodiment 1

[0038] The present invention will be described in further detail below in conjunction with the examples, but the protection scope of the present invention is not limited to the content described. Embodiment 1, a kind of preparation method of lobaplatin trihydrate, concrete operation is as follows:

[0039] (1) Potassium iodoplatinite synthesis process

[0040] Add 10.0 g of potassium chloroplatinite to water for dissolution, and another potassium iodide with a molar ratio of 1:5 to potassium chloroplatinite is added to water for dissolution. The two solutions are mixed and stirred at 20°C for 2.0 hours in the dark. Wherein, potassium chloroplatinite: water is 1g: 1mL, potassium iodide: water is 1g: 1mL, and the dissolution temperature is 40°C.

[0041] (2) Synthesis process of cis-diiodo-(trans-1,2-diaminomethyl-cyclobutane) platinum(Ⅱ) crude product

[0042] Weigh trans-1,2-diaminomethyl-cyclobutane hydrochloride according to the molar ratio of potassium chloroplatinite to ...

Embodiment 2

[0059] Embodiment 2, a kind of preparation method of lobaplatin trihydrate, concrete operation is as follows:

[0060] (1) Potassium iodoplatinite synthesis process

[0061] Add 100.0 g of potassium chloroplatinite to water for dissolution, and another potassium iodide with a molar ratio of 1:6 to potassium chloroplatinite is added to water for dissolution. The two solutions are mixed and stirred for 1.0 h at 30°C in the dark. Wherein, potassium chloroplatinite: water is 1g: 5mL, potassium iodide: water is 1g: 3mL, and the dissolution temperature is 50°C.

[0062] (2) Synthesis process of cis-diiodo-(trans-1,2-diaminomethyl-cyclobutane) platinum(Ⅱ) crude product

[0063] Weigh trans-1,2-diaminomethyl-cyclobutane hydrochloride according to the molar ratio of potassium chloroplatinite to trans-1,2-diaminomethyl-cyclobutane hydrochloride 1:1.5 , Weigh potassium hydroxide according to the molar ratio of trans-1,2-diaminomethyl-cyclobutane hydrochloride to potassium hydroxide 1:1...

Embodiment 3

[0079] Embodiment 3, a kind of preparation method of lobaplatin trihydrate, concrete operation is as follows:

[0080] (1) Potassium iodoplatinite synthesis process

[0081] Add 1000.0 g of potassium chloroplatinite to water for dissolution, and another potassium iodide with a molar ratio of 1:8 to potassium chloroplatinite is added to water for dissolution. The two solutions are mixed and stirred at 40°C in the dark for 0.5 h. Wherein, potassium chloroplatinite: water is 1g: 10mL, potassium iodide: water is 1g: 5mL, and the dissolution temperature is 60°C.

[0082] (2) Synthesis process of cis-diiodo-(trans-1,2-diaminomethyl-cyclobutane) platinum(Ⅱ) crude product

[0083] Weigh trans-1,2-diaminomethyl-cyclobutane hydrochloride according to the molar ratio of potassium chloroplatinite to trans-1,2-diaminomethyl-cyclobutane hydrochloride 1:1.8 , Weigh sodium oxide according to the molar ratio of trans-1,2-diaminomethyl-cyclobutane hydrochloride to sodium oxide 1:1.8, accordin...

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Abstract

The invention discloses a preparation method of lobaplatin trihydrate, which comprises the following steps: by using potassium chloroplatinite, potassium iodide and trans-1,2-diaminomethylcyclobutanehydrochloride as raw materials and water as a solvent, replacing potassium chloroplatinite with potassium iodo-platinite, and reacting potassium iodo-platinite with trans-1,2-diaminomethylcyclobutanewhich is dissociated from the 1,2-diaminomethylcyclobutane hydrochloride under an alkaline condition through neutralization to generate a diiodide; and refining the diiodide, carrying out hydrolysis reaction on the refined diiodide and silver nitrate, filtering out generated silver iodide precipitate, reacting filtrate with sodium lactate to generate a lobaplatin anhydrous substance, and recrystallizing the lobaplatin anhydrous substance in an acetone-water mixed solvent to obtain the lobaplatin trihydrate. The method has the advantages of short synthesis time and simple operation, the precursor chemical acetone involved in the reaction process can be recycled, and the obtained lobaplatin trihydrate has the advantages of high purity, high yield and good stability, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of lobaplatin trihydrate, which belongs to the field of chemical synthesis. Background technique [0002] Lobaplatin (lobaplatin), also known as Lobaplatin and Lobaplatin, has a chemical name of 1,2-diaminomethyl-cyclobutane-lactate platinum (II), and its trihydrate chemical structure is as follows: [0003] [0004] Since the successful development of Lobaplatin, it has been nearly 30 years of development. Among them, the patent CN1120046A found through research and comparison that Lobaplatin anhydrous is easy to deliquesce and become sticky, difficult to make preparations, unrepeatable and controllable water content, stable Poor stability, poor purity and content repeatability, etc., and then proposed a preparation method of lobaplatin trihydrate, the obtained lobaplatin trihydrate can obviously improve the problems caused by lobaplatin anhydrate, and has the advantages of stability, easy storage, Eas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
CPCC07F15/0093Y02P20/55
Inventor 刘其星丛艳伟谢丽娇张林涛王应飞陈红娟郭明里李金伟
Owner KUNMING GUIYAN PHARMA
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