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Preparation method of cyromazine

A technology of cyromazine and diamino, which is applied in the field of preparation of veterinary medicine and pharmaceutical raw material drug cyromazine, and can solve the safety hazards and disadvantages of 2-cyclopropylamino-4,6-dichloro-S-triazine Safe production and environmental protection, shortening the response time and other issues, to achieve the effect of solving the contradiction between economic production and environmental protection, strong practical production technology, and significant economic benefits

Active Publication Date: 2020-09-04
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is an intermediate in these preparation methods, i.e. 2-cyclopropylamino-4,6-dichloro-S-triazine, which has the disadvantages of high toxicity and easy sensitization, which is not conducive to safe production and environmental protection
There are also researchers who use xylene as the reaction solvent to isolate the reaction materials from the environment, and add ethanol in the ammoniation step to shorten the reaction time. Although the yield is increased to 88%, there are also 2-cyclopropylamino-4,6 -The safety hazard of dichloro-S-triazine, similarly, in the final product formation step, use autoclave and ammonia gas, carry out the ammoniation reaction under high temperature 105~135 ℃, pressurization 1.2~1.7Mpa, cause production process there is a certain risk in

Method used

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  • Preparation method of cyromazine
  • Preparation method of cyromazine
  • Preparation method of cyromazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 20.05g of melamine, add it to 100.20g of hydrochloric acid aqueous solution with a pH value of 4, start stirring, and raise the temperature to 100°C. During the reaction, 1M hydrochloric acid is continuously added to maintain the pH value, and the reaction is carried out for 7 hours. Then add 1M sodium hydroxide to adjust the reaction system to a pH value of about 7.0, then cool down to 5°C, filter, and dry to obtain 20.23g of solid, the main component of which is 4,6-diamino-2-hydroxy-1,3 ,5-triazine with a purity of 96.13%.

[0025] All the products obtained above were added to 80.65g of toluene, and the temperature of the system was lowered to 5°C. Within 0.5h, 21.87g of thionyl chloride was added dropwise, and the temperature was controlled at 5-10°C. After the dropwise addition was completed, the temperature was raised to 65° C. and kept for 30 minutes. During the chlorination reaction process, acid gas will be released, so attention should be paid to tail ga...

Embodiment 2

[0028] Take 20.13g of melamine, add it to 100.05g of hydrochloric acid aqueous solution with a pH value of 3.5, start stirring, and raise the temperature to 100°C. During the reaction, 1M hydrochloric acid is continuously added to maintain the pH value, and the reaction is carried out for 7 hours. Then add 1M sodium hydroxide to adjust the reaction system to a pH value of about 7.0, then cool down to 5°C, filter, and dry to obtain 20.30 g of solids, the main component of which is 4,6-diamino-2-hydroxy-1,3 ,5-triazine with a purity of 95.46%.

[0029] All the products obtained above were added to 80.39g of toluene, and the temperature of the system was lowered to 5°C. Within 0.5h, 21.79g of thionyl chloride was added dropwise, and the temperature was controlled at 5-10°C. After the dropwise addition was completed, the temperature was raised to 63° C. and kept for 30 minutes. During the chlorination reaction process, acid gas will be released, and attention should be paid to ab...

Embodiment 3

[0032] Take 20.03g of melamine, add it to 100.15g of hydrochloric acid aqueous solution with a pH value of 4.5, start stirring, and raise the temperature to 100°C. During the reaction, 1M hydrochloric acid is continuously added to maintain the pH value, and the reaction is carried out for 7 hours. Then add 1M sodium hydroxide to adjust the reaction system to a pH value of about 7.0, then cool down to 5°C, filter, and dry to obtain 20.17g of solid, the main component of which is 4,6-diamino-2-hydroxy-1,3 ,5-triazine with a purity of 94.96%.

[0033] All the products obtained above were added to 80.37g of toluene, and the temperature of the system was lowered to 5°C. Within 0.5h, 21.54g of thionyl chloride was added dropwise, and the temperature was controlled at 5-10°C. After the dropwise addition was completed, the temperature was raised to 61° C. and kept for 30 minutes. During the chlorination reaction process, acid gas will be released, so the exhaust gas should be absorbe...

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Abstract

The invention discloses a preparation method of cyromazine. Melamine is used as an initial raw material; the preparation method comprises the following steps: carrying out an acidic hydrolysis reaction to obtain 4, 6-diamino-2-hydroxy-1, 3, 5-triazine, carrying out a chlorination reaction on 4, 6-diamino-2-hydroxy-1, 3, 5-triazine to obtain a toluene solution of 4, 6-diamino-2-chloro-1, 3, 5-triazine, and carrying out an amination reaction on 4, 6-diamino-2-chloro-1, 3, 5-triazine and cyclopropylamine so as to generate cyromazine. According to the method, toxic 2-cyclopropylamino-4, 6-dichloro-S-triazine is prevented from being generated, ammoniation pressurizing equipment is prevented from being used, reaction conditions are milder, cheaper materials are used, and the prepared cyclopropylamine is high in yield and good in quality.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a preparation method of cyromazine, a veterinary drug and a pharmaceutical raw material drug. Background technique [0002] Cyromazine, chemically called 2-cyclopropylamino-4,6-diamino-1,3,5-triazine, also known as cyromazine, was first developed by Ciba-Geigy Corporation, FDA (U.S. Food and Drug Administration) Drug Administration) and EPA (U.S. Environmental Protection Association) officially approved the production of new pesticides in 1974. In recent years, the drug has been widely used in animal husbandry, and the effect is remarkable. [0003] According to literature reports, the traditional synthesis process of cyromazine has many steps and takes a long time. It is generally divided into three steps, and the second and third step reaction times are relatively long, requiring a total of 36 to 48 hours, and the product yield is low. In the pat...

Claims

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Application Information

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IPC IPC(8): C07D251/70
CPCC07D251/70
Inventor 程贺董真奇段良鹏王兴国
Owner SHANDONG GUOBANG PHARMA
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