Method of cis-dichlorodimethylaminoplatinum (ii) obtainment

FIELD: pharmacology.

SUBSTANCE: invention can be applied in medicine and pharmaceutics. Bioactive cis-dichlorodimethylaminoplatinum (II) is obtained by heating aqueous solution containing potassium tetrachloroplatinate (II), methylaminochloride and potassium acetate to 80°C for 4 hours.

EFFECT: cis-dichlorodimethylaminoplatinum (II) output reaching 69%, admixtures not detected.

4 ex

 

The invention relates to methods of obtaining pure compounds of platinum(II), in particular CIS-dichlorodiammineplatinum(II), which has biological activity and exerts its anticancer properties.

Described as ways of obtaining this compound [1-4].

Method [1] based on the reactions:

To2[PtCl4]+4 KI=K2[PtI4]+4 KS1

To2[PtI4]+2 CH3NH2=CIS-[Pt(CH3NH2)2I2]+2 KI

CIS-[Pt(CH3NH2)2I2]+2AgNO3+2H2O=CIS-[Pt(CH3NH2)2(H2O)2](NO3)2+2AgI↓

CIS-[Pt(CH3NH2)2(H2O)2](NO3)2+2KCl=CIS-[PT(CH3NH2)2CL2]+2KNO3+2H2About

In the method [2] CIS-[Pt(CH3NH2)2Cl2] get reactions, which are described in [1], but instead of the use of potassium iodide potassium bromide, and instead of potassium chloride is used hydrochloric acid.

Method [3] includes the interaction of K2[PtCl4] with KI and the subsequent addition of methylamine and isolation of CIS-[Pt(CH3NH2)2I2], excluding the stage of getting To2[PtI4], and further synthesis are similar to the way [1]. In the same paper [3] describes another method of obtaining CIS-[Pt(CH3NH2)2Cl2] from kompleksnog the compounds CIS-[Pt(CH 3NH2)2Cl4based on the reactions:

CIS-Pt(CH3NH2)2I2]+7l2+6N2O=CIS-[Pt(CH3NH2)2Cl4]+NO3+10l

2 CIS-[PT(CH3NH2)2CL4]+N2H6SO4=2 CIS-[Pt(CH3NH2)2Cl2]+H2SO4+4l+N2

The output of the main product by the method [2] is 34% of the K2[PtBr4]and method [3] does not exceed 50% of the K2[PtCl4].

Closest to the claimed is a method for CIS-dichlorodiammineplatinum(II), including the interaction of tetrachloroplatinate(II) potassium with methylamine in acetate-chloride environments during heating [4]. 4 g K2[PtCl4] dissolved in 40 ml of water and, if necessary, filtered. Separately in 20 ml of water successively dissolve 3 g of CH3NH2·HCl, 4,36 g CH3The Cooke and 0.68 g of KCl. The second solution is poured into a solution of platinite potassium and heated to boiling. Thus begins a rich selection of metallic platinum, which quickly separated on the filter. The hot filtrate continue to boil and re-released platinum quickly separated through the same filter. Through 1-1,5 hours there has been a gradual change in color of the solution, the amount of released metal platinum is reduced. The last yellow filtrate evaporated on the water is Noah bath prior to the formation of crystals on the surface and leave it for 3-4 hours or the whole night. A mixture is formed of crystals of [Pt(CH3NH2)2Cl2] and KCl, which after separation dissolved in perhaps a smaller amount of water when heated in a water bath and left for crystallization. Gradually, as the cooling solution is formed crystalline precipitate lemon-yellow color, which is 2 hours can be filtered. Output ≈0.7 g or 22% of theoretical.

The disadvantage of this method, like the previous one, is the low yield of the main product 22%, 34% and 50%, respectively. Synthesis of [4] is carried out at the boiling solution, so more than half the original complex decomposes to metallic platinum. In synthesis [2, 3] used a solution of AgNO3that may partly remain as impurities in the final product.

The aim of the invention is to increase the yield and purity of the CIS-dichlorodiammineplatinum(II).

This goal is achieved:

- the use of high-purity complex compounds of tetrachloroplatinate(II) potassium, synthesized by our method [5],

- increase the yield and purity of the salt of CIS-dichlorodiammineplatinum(II) by creating the optimal ratio of the concentration of the complex in solution and methylamine in concentrated chloride environments.

The essence of the proposed method consists in the following. Salt tetrachloroplatinate(II) dissolved potassium is in an aqueous solution of chloride methylamine and potassium acetate, the solution is heated to 80°C. and reaction are for 4 hours at a given temperature. Released Sol CIS-dichlorodiammineplatinum(II) with small amounts of KCl is filtered off and recrystallized from aqueous solution at room temperature.

The basis of the proposed method to obtain CIS-dichlorodiammineplatinum(II) based on the following new data:

- found conditions of maximum accumulation of CIS-dichlorodiammineplatinum(II) chloride solution of methylamine and potassium acetate depending on the temperature and time of reaction.

- established causes side amination processes and formation of a double salt complexes of platinum(II), minimized their contributions in obtaining the final product.

From the comparison with the prototype shows that the proposed method has the following differences:

the amination reaction is carried out at a temperature of 80°C,

- excluded from the synthesis of the introduction of additional quantities of potassium chloride,

the process is conducted without evaporation,

- the result is an increase in the yield and purity of product CIS-dichlorodiammineplatinum(II) to 69%.

Example 1. To 10 g of K2[PtCl4] (2,41·10-2mol) was added 1 g of CH3NH2·HCl (1,12·10-2mol) and 10 g of CH3The Sook (1,0·10-2mol), dissolved in 40 ml of water. The solution is heated at 80°C in ECENA 4 hours, until it turns yellow. Then, if necessary, it is filtered and cooled to room temperature and leave for 3-4 hours. The resulting precipitate CIS-dichlorodiammineplatinum(II) with small amounts of KCl is dissolved in 30 ml of water by heating on a water bath and left to crystallize at room temperature for 2 hours. The precipitate is filtered off, washed with alcohol and dried. The amount of released complex CIS-[Pt(CH3NH2)2Cl2] - 5.5 g, representing 69% of theoretical. Compound CIS-[PT:(CH3NH2)2CL2] characterized by the following methods: elemental analysis, Rst, IR and UV spectroscopy. Received data Rst and IR spectroscopy coincide with the literature [6, 7]. Impurities [Pt(CH3NH2)4]·[PtCl4] and KCl was not found.

Example 2. To 10 g of K2[PtCl4] (2,41·10-2mol) was added 1 g of CH3NH2·HCl (1,12·10-2mol) and 10 g of CH3The Sook (1,0·10-2mol), dissolved in 40 ml of water. The solution is heated at 90°C for 3.5 hours until it turns yellow. Then the resulting small amount of metallic platinum is filtered and cooled to room temperature and leave for 3-4 hours. The resulting precipitate CIS-dichlorodiammineplatinum(II) with small amounts of KCl is dissolved in 30 ml of water, ringrevenue in a water bath and left to crystallize at room temperature for 2 hours. The precipitate is filtered off, washed with alcohol and dried. The amount of released complex CIS-[Pt(CH3NH2)2Cl2] - 3,71 g, which is 47% of theoretical.

Compound CIS-[PT(CH3NH2)2CL2] characterized by the following methods: elemental analysis, Rst, IR and UV spectroscopy. Impurities [Pt(CH3NH2)4]·[PtCl4] and KCl was not found.

Example 3. To 15 g of K2[PtCl4] (3,61·10-2mol) is added 17 g of CH3NH2·HCl (2,52·10-2mol) and 15 g of CH3The Sook (1,58·10-2mol), dissolved in 60 ml of water. The solution is heated at 80°C for 3 hours, until it turns yellow. Then the resulting small amount of metallic platinum is filtered and cooled to room temperature and leave for 3-4 hours. The resulting precipitate CIS-dichlorodiammineplatinum(II) with small amounts of KCl is dissolved in 30 ml of water by heating on a water bath and left to crystallize at room temperature for 2 hours. The precipitate is filtered off, washed with alcohol and dried. The amount of released complex CIS-[Pt(CH3NH2)2Cl2] - 7,00 g, which is 59% of theoretical. Compound CIS-[Pt(CH3NH2)2Cl2] characterized by the following methods: elemental analysis, Rst, IR and UV spectroscopy. Impurities [Pt(CH3NH2)4]·[PtCl4] and KCl was not found.

Example 4. To 15 g of K2[PtCl4] (3,61·10-2mol) is added 17 g of CH3NH2·HCl (2,52·10-2mol) and 15 g of CH3The Sook (1,58·10-2mol), dissolved in 60 ml of water. The solution is heated at 80°C for 7 hours, until it turns yellow. Then the resulting small amount of metallic platinum is filtered and cooled to room temperature and leave for 3-4 hours. The resulting precipitate CIS-dichlorodiammineplatinum(II) with small amounts of KCl is dissolved in 30 ml of water by heating on a water bath and left to crystallize at room temperature for 2 hours. The precipitate is filtered off, washed with alcohol and dried. The amount of released complex CIS-[Pt(CH3NH2)2Cl2] - 8,48 g, which is 72% of theoretical. Compound CIS-[Pt(CH3NH2)2Cl2] characterized by the following methods: elemental analysis, Rst, IR and UV spectroscopy. Found admixture of [Pt(CH3NH2)4]·[PtCl4].

Example 1 shows the optimal conditions for obtaining the complex CIS-dichlorodiammineplatinum(II) as the concentration of platinum in the solution, and the purity and yield of the main product. Changing the initial concentration of the complex in solution in strenuosity will lead to an increase in the concentration of chloride ion in the solution, and contamination of the core product potassium chloride and reducing output of CIS-[Pt(CH 3NH2)2Cl2]. The decrease in the initial concentration of the complex in solution will lead to a reduction of yield of the main product. The temperature increase in the synthesis leads to contamination of the main product platinum mobile, potassium chloride and reducing output (example 2). The increase in the concentration of methylamine in the synthesis is accompanied by deeper process amination complexes of platinum(II) in solution, which reduces the yield of the main product (example 3). The decrease in the concentration of methylamine in solution leads to longer reaction and contamination of the primary product of the double salt [Pt(CH3NH2)4]·[PtCl4] (example 4).

Thus, this method allows to obtain a salt of CIS-dichlorodiammineplatinum(II) with great output (example 1).

The way to obtain CIS-dichlorodiammineplatinum(II) from aqueous solution tetrachloroplatinate(II) potassium using chloride methylamine and potassium acetate when heated, characterized in that the solution tetrachloroplatinate(II) of potassium are heated with chloride methylamine in potassium acetate solution for 4 h at 80°C without the introduction of additional quantities of potassium chloride and without the process of evaporation, recrystallization is carried out at room temperature.



 

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