Method for preparing cyromazine

A technology of cyromazine and ammonia water, which is applied in the field of veterinary drugs and pesticides, can solve the problems of high risk factor, hidden safety hazard, flammability and explosion, etc., and achieve the effect of high safety factor, pollution avoidance and good stability

Active Publication Date: 2018-05-29
河南后羿制药有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

The disadvantage of this method is that the use of acetone and ethanol in industrial production has a high risk fact

Method used

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  • Method for preparing cyromazine
  • Method for preparing cyromazine
  • Method for preparing cyromazine

Examples

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Embodiment 1

[0031] A preparation method for cyromazine, comprising the following steps:

[0032] 1) Dissolve 30g of cyanuric chloride in 155g of trichlorethylene at 0°C under stirring conditions, and add dropwise 60g of 25% industrial ammonia water; heat up to 40°C, react for 6 hours to obtain a reaction solution, and under the same temperature conditions , after separating trichlorethylene by vacuum distillation, add 180g of purified water, stir for 1 hour, then lower to 25°C, filter with suction, wash with water, and dry in vacuum for 8h at 50°C to obtain 22.5g of intermediate, which is 2-chloro -4.6-diamino-1.3.5-triazine dry product, the mass yield of the intermediate is 95%;

[0033] 2) Add 165ml of purified water to 22.5g of the intermediate in step 1, then add 10.5g of cyclopropylamine, heat up to 90°C, add dropwise an aqueous solution of sodium carbonate (an aqueous solution prepared by dissolving 8.8g of sodium carbonate in 27ml of purified water), Adjust pH=7.5-8.5, keep warm f...

Embodiment 2

[0035] A preparation method for cyromazine, comprising the following steps:

[0036] 1) Dissolve 20g of cyanuric chloride in 120g of 1,2-dichloroethane at 5°C under stirring condition, add dropwise 40g of 25% industrial ammonia water; heat up to 45°C, react for 6h to obtain a reaction solution, Under the same temperature conditions, after vacuum distillation and separation of 1,2-dichloroethane, 120g of purified water was added, stirred for 1 hour, then lowered to 25°C, filtered with suction, washed with water, and vacuum-dried at 55°C for 6h to obtain 14.8g Intermediate, the intermediate is a dry product of 2-chloro-4.6-diamino-1.3.5-triazine, and the mass yield of the intermediate is 94%;

[0037] 2) Add 120ml of purified water to the intermediate of step 1), then add 7.2g of cyclopropylamine, heat up to 95°C, add dropwise an aqueous solution of potassium carbonate (an aqueous solution prepared by dissolving 7.8g of potassium carbonate in 28ml of purified water), and adjust ...

Embodiment 3

[0039] A preparation method for cyromazine, comprising the following steps:

[0040] 1) Dissolve 30 g of cyanuric chloride in 160 g of 1,2-dichloroethane at 3° C. under stirring, and dropwise add 60 g of 25% industrial ammonia water; raise the temperature to 42° C., and react for 6 hours to obtain a reaction solution. Under the same temperature conditions, after vacuum distillation and separation of 1,2-dichloroethane, 180g of purified water was added, stirred for 1 hour, then lowered to 25°C, suction filtered, washed with water, and vacuum-dried at 52°C for 7h to obtain 22.8g Intermediate (dry product of 2-chloro-4.6-diamino-1.3.5-triazine), the mass yield of the intermediate is 96%;

[0041] 2) Add 170ml of purified water to the intermediate in step 1), then add 10.8g of cyclopropylamine, heat up to 92°C, add dropwise an aqueous solution of potassium carbonate (an aqueous solution prepared by dissolving 9.0g of potassium carbonate in 30ml of purified water), Adjust pH=7.5-8...

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Abstract

The invention discloses a method for preparing cyromazine. The method includes steps of 1), dissolving cyanuric chloride in organic solvents under stirring conditions at the temperature of 0-5 DEG C,then dropwise adding industrial ammonia water into the organic solvents to obtain mixtures, heating the mixtures until the temperatures of the mixtures reach 40-45 DEG C, carrying out thermal reactionfor 5-6.5 h to obtain reaction liquid, separating solvents from the reaction liquid, adding purified water into residual liquid, stirring the purified water and the residual liquid for 1-1.5 h to obtain mixed liquid, cooling the mixed liquid until the temperature of the mixed liquid reaches the room temperature and carrying out suction filtration, washing and drying to obtain an intermediate which is 2-chlorine-4.6-diamino-1.3.5-triazine; 2), adding the intermediate prepared at the step 1) into purified water at the room temperature, adding cyclopropylamine into the purified water to obtain first mixtures, heating the first mixtures until the temperatures of the first mixtures reach 90-95 DEG C, dropwise adding acid binding agents into the first mixtures to obtain second mixtures, regulating the pH (potential of hydrogen) of the second mixtures until the pH of the second mixtures reaches 7.5-8.5, then carrying out reaction at the temperature of 98-100 DEG C for 3.5-4.5 h, carrying outdecolorization and filter to obtain reaction solution, cooling the reaction solution until the temperature of the reaction solution reaches 40-50 DEG C, crystallizing the reaction solution for 1-2 h,continuing to cool crystals until the temperatures of the crystals range from -5 DEG C to 0 DEG C, carrying out suction filtration and washing and then carrying out drying to obtain the cyromazine. The method has the advantages that the method includes simple processes and is high in safety and low in cost, and industrial production can be facilitated; the cyromazine which is a product is high inpurity, low in impurity content and good in stability.

Description

technical field [0001] The invention belongs to the technical field of pesticides and veterinary drugs, and in particular relates to a preparation method of cyromazine. Background technique [0002] Cyromazine (Cyromazine) is a triazine compound, the chemical name is 2-cyclopropylamino-4,6-diamino-1,3,5-triazine (N-Cyclopropyl-1,3,5- triazine-2,4,6-triamine), which has the characteristics of insect growth regulation and insecticidal specificity, can be degraded by microorganisms, has no residual toxicity, is safe to use, and does not pollute the environment. It is a new type of high-efficiency, low-toxic, nitrogen-containing heterocycle Insecticides, also known as cyromazine because it also has a fly-killing effect. [0003] At present, the method for preparing cyromazine mainly contains following several kinds: [0004] 1) With cyanuric chloride, cyclopropylamine, industrial ammonia (20%) and liquid ammonia as raw materials, three-step synthesis of cyromazine, the synthet...

Claims

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Application Information

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IPC IPC(8): C07D251/70C07D251/50
CPCC07D251/50C07D251/70
Inventor 张华刚万毅李贵欣
Owner 河南后羿制药有限公司
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