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The preparation method of azimidone

A technology for mezotrione and triazinon is applied in the field of preparation of mezotrione, can solve problems such as being difficult to remove, and achieve the effects of ensuring product purity, improving reaction selectivity, and improving reactivity

Active Publication Date: 2022-01-07
JIANGSU REPONT PESTICIDE FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The S-methylation reaction produces the target product, metrizone, and the N-methylation reaction produces impurities, which can form a co-crystal with the target product, making it difficult to remove

Method used

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  • The preparation method of azimidone
  • The preparation method of azimidone
  • The preparation method of azimidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0034] The preparation method of the namazone of the present embodiment includes the following steps:

[0035] Mechanical stirring is installed on 1000 ml of four bottles, and the air-conditioned guiding tube, thermometer and condenser are not entered. 21 g (0.88 mol) of lithium hydroxide solids and 600 ml of water were added to a four-mouth bottle, and after stirring for lithium hydroxide, 200 ml of methanol was added to the bottle.

[0036] Control the temperature of 15 ° C to 20 ° C in the bottle, slowly add 160 g (0.8 mol) triazide (4-amino-6-tert-butyl-3-thiol-1,2,4-triazine -5) with stirring. Ketone), stirred and dissolved.

[0037] The bromomethane gas was introduced into the bottle, and the lithium hydroxide solution of 2 mol / L was added dropwise as the passage of bromomethane gas was slowly added dropwise to maintain a pH of the reaction system of 11.5 to 12.5, and liquid chromatography was tracked. The triazinone completely disappears (the reaction ends in this example...

Embodiment 2）

[0049] The preparation method of the namazone of the present embodiment includes the following steps:

[0050] Mechanical stirring is installed on 1000 ml of four bottles, and the air-conditioned guiding tube, thermometer and condenser are not entered. Was added solid lithium hydroxide and 21g water 600mL four-neck flask, lithium hydroxide was stirred until complete dissolution, methanol was added 200mL bottle.

[0051] Controlling inner temperature 15 ℃ ~ 20 ℃, under stirring slowly added 160g triazin-one (4-amino-6-tert-butyl-3-mercapto-1,2,4-triazin-5-one), stirred a clear solution.

[0052] Was slowly passed through the chloride gas bottle, and passed as methyl chloride gas was slowly added dropwise 2 mol / L lithium hydroxide solution to maintain the pH value of the reaction system, 11.5 to 12.5, with the sample liquid chromatography tracking complete disappearance of the triazine-one (Example 14 of the present embodiment the end of the reaction to 16 hours); inner temperatur...

Embodiment 3）

[0055] The preparation method of the namazone of the present embodiment includes the following steps:

[0056] Mechanical stirring is installed on 1000 ml of four bottles, and the air-conditioned guiding tube, thermometer and condenser are not entered. 34g solid sodium hydroxide, lithium 37g (0.87 mol) solid chloride and water were added 600mL four-necked flask, stirring until completely dissolved, methanol was added 200mL bottle.

[0057] Controlling inner temperature 10 ℃ ~ 15 ℃, was slowly added with stirring 160g triazin-one (4-amino-6-tert-butyl-3-mercapto-1,2,4-triazin-5-one), stirred a clear solution.

[0058] Slowly to the methyl bromide gas into the bottle, and with the methyl bromide gas is passed slowly added dropwise 2 mol / L sodium hydroxide solution, the reaction system to maintain a pH value of 11.5 to 12.5, with the sample tracking liquid chromatography complete disappearance of the triazine-one (Example 5 of the present embodiment the end of the reaction to 6 hou...

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Abstract

The invention discloses a method for preparing metrizone. Using methanol-water as a solvent, in the presence of pH 11.5-12.5 and lithium ions, triazinone and methyl halide react at 5°C-20°C to three Azinones disappear completely. The present invention adds lithium ions to the reaction system during the preparation of mecitrione, which improves the selectivity of the reaction to produce mecitrione. The addition of lithium ions improves the ability of triazinone to exist in the form of thiols, thereby increasing the concentration and reactivity of sulfide anions in the reaction system, and the generated products are mainly S-methylated products, reducing impurities N-methyl Therefore, there is basically no impurity in the product, and the purity of mecitrione is more than 99%.

Description

Technical field [0001] The present invention relates to a method of preparation of zyzazone. Background technique [0002] Nazazin ketone (Metribuzin, 4-amino-6-Triazine-3-methylthio-1,2,4-triazine-5 (4H)-ketone) is a triazinketone by DuPont Company Herbic, product name Syaken, LEXONE, MISTRAL, etc. Wait. [0003] The mechanism of action of zinazone is: namazone is absorbed by the thromid root resistance, which can be conducted in the upper portion of the transpiration, or the leaf absorbed in the body is limited, and the graft is used to play a killing activity by suppressing photosynthesis of sensitive plants. After the application, various sensitive weeds were unaffected, and the leaves were faded after the seedling. In the final nutrition and dried, the symptoms were green vane or fire, and the entire leaf can be changed, but the vein is often residual. Interlaced green. [0004] There are many patents and journal documents for the preparation method of zixazoids, which have ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D253/075
CPCC07D253/075
Inventor 杨晓放步康明步杰颜建忠汪兴园秦文华步成伟胡俊
Owner JIANGSU REPONT PESTICIDE FACTORY
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