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Synthesis process of triazine amide

A technology of triazine amide and synthesis process, which is applied to the field of synthesis technology of intermediates, can solve the problems of high cost, high solution toxicity and high energy consumption, and achieves the effects of improving yield, shortening reaction time and improving reaction yield

Inactive Publication Date: 2012-06-13
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The production process of this method is quite mature, but there are also disadvantages such as high energy consumption, high solution toxicity, and high cost. Therefore, it is very useful to optimize the synthesis process of triazinamide to achieve the purpose of increasing yield and reducing cost. necessary

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1320g of toluene was added into the four-necked reaction flask, and 264g of oxadiazolone was added under the condition of stirring. After the addition, continue stirring for 21 minutes, heat up to 54°C, start to drop 237.6 g of chloroacetone, and reflux at 50-51°C for 6 hours. Sampling analysis, 20 minutes to reach the end. Turn on the vacuum to remove toluene and chloroacetone. Add 1320g of ethanol, 158g of hydrazine hydrate (content 80%) and 20g of anhydrous sodium sulfate, react at 76-79°C for 6.2 hours, cool and crystallize, filter with suction, wash and dry to obtain triazinamide, and the reaction yield is 84%.

Embodiment 2

[0025] 1320g of toluene was added into the four-necked reaction flask, and 264g of oxadiazolone was added under the condition of stirring. After the addition, continue stirring for 22 minutes, heat up to 55°C, start to drop 237.6 g of chloroacetone, and reflux at 53-55°C for 3.5 hours. Sampling analysis, 50 minutes to reach the end. Turn on the vacuum to remove toluene and chloroacetone. Add 1320g of ethanol, 158g of hydrazine hydrate and 60g of anhydrous sodium sulfate, react at 76-79°C for 8 hours, cool to crystallize, filter with suction, wash and dry to obtain triazine amide, and the reaction yield is 86.1%.

Embodiment 3

[0027] A. Add toluene into the reaction kettle, start stirring, heat, when the temperature rises to 50°C, add oxadiazolone (2-methyl-1,3,4-oxadiazol-5(4H)-one), Add and continue to stir for 15 minutes;

[0028] B. When the temperature is 45°C, add chloroacetone dropwise for reflux reaction, the dropping time is controlled at 3 hours, then continue the reaction at 45°C, and follow up sampling to determine when pH=5 is determined as the end point of the reaction, and the reaction solution is obtained;

[0029] C. Carry out vacuum distillation on the reaction solution obtained in step B, remove toluene and chloroacetone, then add ethanol, hydrazine hydrate and dehydrating agent anhydrous sodium sulfate, heat up to 75°C, react for 6 hours, and slowly cool down to 25°C;

[0030] D. Centrifugal separation, washing and drying to obtain the intermediate triazinamide (4,5-dihydro-4-acetamido-6-methyl-1,2,4-triazin-3-(2H)-one) .

[0031] The reaction feed molar ratio of the present in...

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Abstract

The invention relates to a synthesis process of triazine amide. Oxadiazol ketone (2-mehtyl-1, 3, 4-oxadiazole-5 (4H)-ketone) and chloroacetone are used as raw materials, toluene serves as solvent, and the triazine amide is prepared through cyclization, alkylation and condensation reaction. By adopting thermal insulation dropping reaction, the synthesis process effectively improves service efficiency of a reaction kettle, reduces usage amount of acetone, increases reaction yield, and finally obtains the solid triazine amide (4, 5-dihydro-4-acetamido-6-methyl-1, 2, 4-triazine-3-(2H)-ketone) with total yield of 84% to 86%.

Description

technical field [0001] The present invention relates to a kind of synthetic technology of intermediate, more specifically, the present invention relates to a kind of synthetic technology of triazinamide. technical background [0002] Pymetrozine belongs to pyridine or triazinone insecticides. It is a brand-new non-biocide insecticide. It was first developed by Ciba-Geigy in Switzerland in 1988. Pests showed excellent control effect. [0003] Studies using electropenetrography (EPG) techniques have shown that no matter in drip, feeding or injection experiments, as long as aphids or planthoppers are exposed to pymetrozine, they almost immediately produce a stylet blocking effect, stop feeding immediately, and eventually starve fatal, and the process is irreversible. Therefore, pymetrozine has an excellent function of blocking insect transmission. Although the mechanism of stylet blockage caused by pymetrozine is not yet clear, existing studies have shown that this irreversi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D253/06
Inventor 袁树林阮冬冬罗翔王梅
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD