Method for refining ethylmercurithiosalicylic acid and preparing merthiolate sodium

A technology of thimerosal acid and thimerosal, applied in the field of medicine, can solve the problems of difficulty in achieving high-purity thimerosal sodium, and difficulty in controlling the content of sodium salt.

Inactive Publication Date: 2014-05-07
JIANGXI ZETONG PHARMA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent CN101696219A uses mercuric chloride and monochlorodiethylaluminum as raw materials to prepare chloroethylmercury, and then reacts with sodium thiosalicylate solution to prepare thimerosalic acid, which is directly prepared into sodium salt without refining , the sodium salt content obtained by this method is not easy to control
[0006] East German patent Ger (East) 49843 (1966) discloses a method for preparing sodium thimerosal by salting sodium alkoxide and thimerosalic acid, and it is difficult to achieve high-purity sodium thimerosal without the refining of thimerosalic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of Grignard reagent: fully dry the reactor, pass into nitrogen protection, quickly add 3.24g (0.134mol) magnesium chips, 80ml anhydrous tetrahydrofuran and a little iodine crystal, then, under stirring, slowly and evenly drop in 14.6g ( 0.134kmol) of anhydrous bromoethane, by controlling the dripping speed to control the temperature of the kettle at 20-30°C, the addition is completed in 3-8 hours, after the drop is completed, stir at 30°C for another 2 hours until the magnesium chips disappear, and filter to obtain bromine Ethylmagnesium solution.

[0026] Preparation of ethylmercury halide: fully dry the reactor, blow nitrogen into it, quickly add 36.68 g (0.134 mol) of mercuric chloride and 150 ml of anhydrous tetrahydrofuran and stir at room temperature for half an hour, then, under stirring, mix the Grignard reagent obtained above Add slowly, control the temperature at 20-60°C, and complete the addition in 1-5 hours. After the addition was complete, it ...

Embodiment 2

[0034] Preparation of Grignard reagent: The reactor was fully dried, protected by nitrogen gas, quickly added 3.24g (0.134mol) of magnesium chips, 90ml of anhydrous 2-methyltetrahydrofuran and a little methyl iodide, and then, under stirring, slowly and evenly dripped Add 14.6 g (0.134mol) of anhydrous bromoethane, and control the temperature of the kettle at 20-30°C by controlling the dripping speed, and add it in 3-8 hours. After the drop is complete, stir at 30°C for another 2 hours until the magnesium chips disappear. , and filtered to obtain ethylmagnesium bromide solution.

[0035] Preparation of ethylmercury halide: fully dry the reactor, feed nitrogen gas, quickly add 36.68 g (0.134 mol) of mercury chloride and 180 ml of anhydrous 2-methyltetrahydrofuran and stir at room temperature for half an hour, then, under stirring, the above-mentioned Add the Grignard reagent slowly, control the temperature at 20-60°C, and complete the addition in 1-5 hours. After the addition ...

Embodiment 3

[0040] The preparation of thimerosalic acid crude product: method is the same as embodiment 1.

[0041] Purification of thimerosalic acid: Add 10.0g of crude thiomersalic acid, 1.0g of activated carbon and 30L of 55% ethanol to the reactor, heat at 60-70°C for 30 minutes and then filter while it is hot. Slowly cool the filtrate to room temperature and then cool down to 0 After crystallization at -5°C for 10 hours, filter and dry in vacuo to obtain 9.1 g of refined thimerosalic acid. Measured melting point: 112-113.5°C.

[0042] The preparation of sodium thimerosalate: method is with embodiment 1.

[0043] 39g sodium thimerosalate was obtained with a yield of 92.6%. The measured content is: 98.0%, melting point: 232-233°C.

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Abstract

The invention relates to a method for refining ethylmercurithiosalicylic acid and preparing merthiolate sodium. The purity of a product is improved through refining crude ethylmercurithiosalicylic acid and then preparing a sodium salt. The method comprises the following steps: enabling mercuric chloride and an ethylmagnesium bromide grignard reagent to react to obtain halogenated ethylmercury; enabling the halogenated ethylmercury and sodium tiosalicylate to react under the protection of nitrogen gas and under the condition that the PH value is larger than 8-9 to obtain crude ethylmercurithiosalicylic acid, wherein the halogenated ethylmercury is obtained in the former step; recrystallizing crude ethylmercurithiosalicylic acid to obtain refined ethylmercurithiosalicylic acid; enabling refined ethylmercurithiosalicylic acid and sodium-contained alkaline or salt to react to prepare merthiolate sodium with high purity. Merthiolate sodium prepared by using the method provided by the invention is high in purity and yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicine, relates to the preparation of thimerosalic acid and its sodium salt, and further relates to a refining method of thimerosalic acid. Background technique [0002] Sodium thimerosal is an effective disinfectant, which can be used for disinfection of skin and mucous membranes, and also for antisepsis of pharmaceuticals. Because of its high efficiency and low toxicity, it is widely used in the fields of pharmaceuticals and cosmetics. The molecular formula of sodium thimerosalate is: [0003] . [0004] Chinese patent CN101696219A uses mercuric chloride and monochlorodiethylaluminum as raw materials to prepare chloroethylmercury, and then reacts with sodium thiosalicylate solution to obtain thimerosalic acid, which is directly prepared into sodium salt without refining , the sodium content of this method gained is difficult to control. [0005] Russian patent Ru2046797 (1993) uses ethyl mercury phosphate...

Claims

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Application Information

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IPC IPC(8): C07F3/12
Inventor 钟劲松周国梁华锋
Owner JIANGXI ZETONG PHARMA CHEM
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