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Environment-friendly synthesis method of medical intermediate dichlorohydantoin

A technology of dichlorohydantoin and green synthesis, applied in the field of medicine and chemical industry, can solve the problems of low reaction efficiency, easy decomposition of sodium hypochlorite, difficult operation, etc., and achieves the effects of improving the reaction rate, reducing side reactions and being easy to obtain.

Inactive Publication Date: 2018-09-04
任伟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Among the above three methods, the sodium hypochlorite used in the first method is easy to decompose, the reaction efficiency is low, and the product content of production is low, and there is no industrialized production; the second method is easy to produce carbon dioxide gas in the reaction process due to the use of sodium carbonate. The process is not easy to operate; the content of liquid caustic soda used in the third method is unstable, generally around 30%, sometimes with a difference of 2%, resulting in unstable content of dichlorohydantoin, generally between 67-69% of available chlorine, sometimes liquid Alkali impurities exceed the standard, affecting product purity
The product obtained by the above several dichlorohydantoin product production methods is low in purity and cannot meet the requirements for use as a pharmaceutical chemical intermediate synthesis. Therefore, it is imperative to develop a high yield and simple synthetic pharmaceutical intermediate dichlorohydantoin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of Nanoscale Ga / Al Composite Solid Base Modified by Lanthanum

[0032] (1) Treat 3g of calcium nitrate and 6g of aluminum nitrate under ultrasonic wave for 3h, then purge at 160°C for 4h under helium atmosphere, and then transfer to a beaker;

[0033] (2) Add 100ml of deionized water into the beaker to dissolve, turn on the magnetic stirring at the same time, and bathe in 100℃ water for 2h;

[0034] (3) Add 8g of kaolin to step (2), stir it with magnetic force, heat it in a water bath to 80°C, and keep it for 3h, then carry out hot alkali treatment, treat it under hot air at 150°C for 2h, and finally transfer it to 200ml with a mass fraction of Treat in 5% sodium hydroxide solution for 6h;

[0035] (4) Transfer the product treated in step (3) to another beaker, add 0.01g of sodium dodecylbenzenesulfonate dropwise, add 80ml of deionized water, put it on a magnetic stirrer for 3 hours, and finally transfer it to the reaction kettle Inside, react at 160kpa, 2...

Embodiment 2

[0047] Preparation of pharmaceutical intermediate dichlorohydantoin

[0048]Get ethyl acetate, tetrahydrofuran and liquid chlorine volume ratio as the sample of 1:1.2:0.5, the nanoscale Ga / Al composite solid alkali mass ratio of 5,5-dimethylhydantoin, anhydrous sodium carbonate and lanthanum modification is 1:1:0.15 sample. 30ml of ethyl acetate, 36ml of tetrahydrofuran, 15ml of liquid chlorine, 7g of 5,5-dimethylhydantoin, 7g of anhydrous sodium carbonate, and 1.05g of lanthanum-modified nano-scale Ga / Al composite solid base. Other raw materials and operation steps are the same with embodiment 1.

Embodiment 3

[0050] Preparation of pharmaceutical intermediate dichlorohydantoin

[0051] Take the sample whose volume ratio of ethyl acetate, tetrahydrofuran and liquid chlorine is 1:1:0.7, the mass ratio of 5,5-dimethylhydantoin, anhydrous sodium carbonate and lanthanum-modified nano-scale Ga / Al composite solid base is 1:1.2:0.13 sample. 30ml of ethyl acetate, 30ml of tetrahydrofuran, 21ml of liquid chlorine, 7g of 5,5-dimethylhydantoin, 8.4g of anhydrous sodium carbonate, and 0.91g of lanthanum-modified nano-scale Ga / Al composite solid base. Other raw materials and operation steps are the same with embodiment 1.

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Abstract

The invention discloses an environment-friendly synthesis method of a medical intermediate dichlorohydantoin. According to the synthesis method, with ethyl acetate and tetrahydrofuran as organic mediaand 5, 5-dimethylhydantoin, liquid chlorine and lanthanum-modified nanoscale Ga / Al composite solid alkali as raw materials, the medical intermediate dichlorohydantoin is obtained through reflux condensation, magnetic stirring and microwave reactor treatment. The unique lanthanum-modified nanoscale Ga / Al composite solid alkali is used for synthesizing the medical intermediate dichlorohydantoin, sothat operation is simple and the raw materials are relatively easy to obtain; through addition of the lanthanum-modified nanoscale Ga / Al composite solid alkali, the reaction rate is effectively increased and occurrence of a side reaction is reduced; in the synthesis process, the smooth progress of the reaction is facilitated and the reaction progresses in a desired direction, so that obtainment of a target product medical intermediate dichlorohydantoin is facilitated.

Description

Technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a green synthesis method of a medicine intermediate dichlorohydantoin. Background technique [0002] The full name of dichlorohydantoin is 1,3-dichloro-5,5-dimethylhydantoin, also known as 1,3-dichloro-5,5-dimethylhydantoin, and its chemical name is 1,3 -Dichloro-5,5-methyl-2,4-imidazolidinedione. [0003] As a new type of high-efficiency disinfectant, dichlorohydantoin has been used in industrial cooling circulating water systems, swimming pool and fountain water disinfection and algae killing, and is also used in aquaculture, animal husbandry and daily life disinfection and sterilization. [0004] At present, the chlorinating agents and oxidizing agents used for the synthesis of pharmaceutical and chemical intermediates generally include chlorine gas, thionyl chloride, phosphorus chloride, chloramine (chloramine T), sodium hypochlorite, trichloroisocyanu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/82B01J23/10
CPCC07D233/82B01J23/10
Inventor 任伟
Owner 任伟