Preparation method of ametryn

Abstract

The invention provides a method for preparing ametryn through a green salt-free technology. The method comprises the following step: under the action of a catalyst, enabling atrazine and methanethiolto react in isopropyl alcohol to prepare the ametryn. According to the method provided by the invention, the production and utilization of sodium thiomethoxide with an offensive odor are avoided; meanwhile, a catalyst with the offensive odor, i.e., trimethylamine hydrochloride, is not used, and the environment-friendly catalyst is used, so that the odor can be avoided radically and the quality ofa product and the environment of a production site are extremely improved; meanwhile, industrial salt is not generated; the method is environmentally friendly and the environment protection cost is greatly reduced.

Description

technical field

[0001] The invention relates to the technical field of pesticides, in particular to a preparation method of ametryn. Background technique

[0002] Ametrine, chemical name: 2-ethylamino-4-isopropylamino-6-methylthio-1,3,5-triazine, English name: atryn, molecular formula: C 9 h 17 N 5 S, molecular weight: 227.33, chemical formula as follows:

[0003]

[0004] Its pure product is white crystal, density: 1.19g / m 3 , melting point 84-86°C, vapor pressure at 20°C is 0.112mPa, solubility in water at 25°C is 200mg / L. It is stable in slightly acidic or slightly alkaline medium, but hydrolyzed into 6-hydroxyl derivatives without herbicidal activity in strong acidic or strongly alkaline medium. It can be mixed with most other pesticides and fertilizers when used in normal doses. The compound is non-flammable, non-explosive and non-corrosive.

[0005] Ametryn is a selective systemic herbicide with rapid herbicidal action. At a low concentration, arazine can pro...

Examples

Embodiment 1

[0039] Fix 1.32g of ZSM-5 catalyst in a 1L autoclave with stirring and temperature controller, add 200g of 97% atrazine, 135.03g of isopropanol, 43.21g of methyl mercaptan, and seal it at a temperature of 90-110°C , stirred and reacted for 1 hour at a pressure of 0.49 to 0.78 to obtain an arazine wet material, which was dried at 105 to 115°C for 1 hour to obtain 206.11 g of an ametryn technical substance, and the arazine content was 99.05 g by HPLC. %, the yield based on atrazine is 99.90%, and the by-product 2-chloropropane is 70.91g, and the content is 99.56%.

[0040] The specific reaction parameters and results are shown in Table 4 and Table 5.

[0041] Weigh respectively the ametryn standard substance and the ametryn original drug prepared in Example 1, and adopt gas chromatography to detect the prepared ametryn original drug, and the results are as follows: figure 1 , figure 2 , Table 1 ~ Table 3 shown.

[0042] Table 1 Gas chromatographic data of the ametryn standar...

Embodiment 2～ Embodiment 10

[0049] The reaction steps are the same as in Example 1, and the specific reaction parameters and results are shown in Table 4 and Table 5.

[0050] Table 4 embodiment 1~10 reaction parameter and result summary

[0051]

[0052]

[0053] Table 5 embodiment 1~10 reaction parameter summary

[0054] Example

[0055] It can be seen from the above examples that the present invention has prepared ametrazine with high yield and purity, and no waste salt is produced in the production process, and the product has no pungent taste.

technical field

[0001] The invention relates to the technical field of pesticides, in particular to a preparation method of ametryn. Background technique

[0002] Ametrine, chemical name: 2-ethylamino-4-isopropylamino-6-methylthio-1,3,5-triazine, English name: atryn, molecular formula: C 9 h 17 N 5 S, molecular weight: 227.33, chemical formula as follows:

[0003]

[0004] Its pure product is white crystal, density: 1.19g / m 3 , melting point 84-86°C, vapor pressure at 20°C is 0.112mPa, solubility in water at 25°C is 200mg / L. It is stable in slightly acidic or slightly alkaline medium, but hydrolyzed into 6-hydroxyl derivatives without herbicidal activity in strong acidic or strongly alkaline medium. It can be mixed with most other pesticides and fertilizers when used in normal doses. The compound is non-flammable, non-explosive and non-corrosive.

[0005] Ametryn is a selective systemic herbicide with rapid herbicidal action. At a low concentration, arazine can pro...

Examples

Embodiment 1

[0039] Fix 1.32g of ZSM-5 catalyst in a 1L autoclave with stirring and temperature controller, add 200g of 97% atrazine, 135.03g of isopropanol, 43.21g of methyl mercaptan, and seal it at a temperature of 90-110°C , stirred and reacted for 1 hour at a pressure of 0.49 to 0.78 to obtain an arazine wet material, which was dried at 105 to 115°C for 1 hour to obtain 206.11 g of an ametryn technical substance, and the arazine content was 99.05 g by HPLC. %, the yield based on atrazine is 99.90%, and the by-product 2-chloropropane is 70.91g, and the content is 99.56%.

[0040] The specific reaction parameters and results are shown in Table 4 and Table 5.

[0041] Weigh respectively the ametryn standard substance and the ametryn original drug prepared in Example 1, and adopt gas chromatography to detect the prepared ametryn original drug, and the results are as follows: figure 1 , figure 2 , Table 1 ~ Table 3 shown.

[0042] Table 1 Gas chromatographic data of the ametryn standar...

Embodiment 2～ Embodiment 10

[0049] The reaction steps are the same as in Example 1, and the specific reaction parameters and results are shown in Table 4 and Table 5.

[0050] Table 4 embodiment 1~10 reaction parameter and result summary

[0051]

[0052]

[0053] Table 5 embodiment 1~10 reaction parameter summary

[0054] Example

[0055] It can be seen from the above examples that the present invention has prepared ametrazine with high yield and purity, and no waste salt is produced in the production process, and the product has no pungent taste.

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