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Preparation method of methoxyfenozide

A technology of methoxyfenozide and dimethylbenzoyl chloride, applied in the field of preparation of methoxyfenozide, can solve the problems of low product yield and content, poor reaction selectivity, difficulty in obtaining high-content intermediates, etc. , to achieve the effects of reducing production costs, environmental friendliness, and product efficiency

Inactive Publication Date: 2018-03-23
SHAANXI QIYUAN TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the present synthetic invention has short reaction steps, it is difficult to obtain high-content intermediates due to the poor reaction selectivity of 3-methoxy-2-methylbenzoyl chloride and tert-butylhydrazine, so the product yield and content low

Method used

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Experimental program
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Effect test

Embodiment 1

[0013] The preparation method of methoxyfenozide of the present invention comprises the following steps:

[0014] The first step, the preparation of 3,5-dimethylbenzoyl chloride, add 3,5-dimethylbenzoic acid and toluene to the reaction flask, raise the temperature to 60°C, add thionyl chloride dropwise within 2 hours, and keep the temperature for 3 hours , and the solvent was removed under reduced pressure to obtain 3,5-dimethylbenzoyl chloride;

[0015] The second step is the synthesis of intermediates. Add tert-butylhydrazine, sodium hydroxide and toluene into the reaction flask, cool to 0°C, add di-tert-butyl dicarbonate, react at 0-5°C for 10h, and separate the water layer. Add 3,5-dimethylbenzoyl chloride and sodium hydroxide aqueous solution to the organic layer, react at 0-5°C for 4h, filter the product, add the filter cake to methanol, add hydrochloric acid to the reaction mixture, react at 35°C for 20h, The product was filtered, washed with water and dried to obtain ...

Embodiment 2

[0018] The preparation method of methoxyfenozide of the present invention comprises the following steps:

[0019] The first step, the preparation of 3,5-dimethylbenzoyl chloride, add 3,5-dimethylbenzoic acid and toluene to the reaction flask, raise the temperature to 60°C, add thionyl chloride dropwise within 2 hours, and keep the temperature for 3 hours , and the solvent was removed under reduced pressure to obtain 3,5-dimethylbenzoyl chloride;

[0020] The second step is the synthesis of intermediates. Add tert-butylhydrazine, sodium hydroxide and toluene into the reaction flask, cool to 0°C, add di-tert-butyl dicarbonate, react at 0-5°C for 10h, and separate the water layer. Add 3,5-dimethylbenzoyl chloride and sodium hydroxide aqueous solution to the organic layer, react at 0-5°C for 4h, filter the product, add the filter cake to methanol, add hydrochloric acid to the reaction mixture, react at 35°C for 20h, The product was filtered, washed with water and dried to obtain ...

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Abstract

The invention discloses a preparation method of methoxyfenozide and relates to the field of insecticide, and particularly relates to the preparation method of methoxyfenozide. The preparation method includes steps of preparation of 3, 5-dimethylbenzoyl chloride: adding 3, 5-mesitylenic acid and methylbenzene in a reaction bottle; raising temperature to 60 DEG C, and dropwise adding thionyl chloride within 2 hours; preserving temperature for 3 hours, depressurizing and removing solvent to obtain 3, 5-dimethylbenzoyl chloride; synthesis of midbody: adding tert-butylhydrazine, sodium hydroxide and methylbenzene in the reaction bottle, and cooling to 0 DEG C; adding di-tert-butyl dicarbonate ester and reacting for 10 hours at 0-5 DEG C; removing a water layer, adding 3, 5-dimethylbenzoyl chloride and sodium hydroxide solution in an organic layer; reacting for 4 hours at 0-5 DEG C, filtering a product and adding the filter cake in methanol; adding hydrochloric acid in the reaction mixture;reacting for 20 hours at 35 DEG C; filtering the product, washing and drying to obtain the midbody. The preparation method is simple in operation, safe and reliable in reaction; the production efficiency is greatly improved, and the production cost is reduced; moreover, the product is high-efficient, low-toxic and environment-friendly.

Description

technical field [0001] The invention relates to the field of insecticides, in particular to a preparation method of methoxyfenozide. Background technique [0002] Methoxyfenozide is a new type of specific phenylhydrazide insecticide with low toxicity, it is effective on vegetables, apples, corn, cotton, grapes, kiwi, walnuts, flowers, sugar beets, tea, rice, sorghum, soybeans and other crops. Lepidoptera pests have highly selective insecticidal activity, mainly contact action, and have certain systemic action. The drug belongs to bionic molting hormones. After the pests eat the drug, they will produce a molting reaction, and the larvae will die due to dehydration and starvation due to incomplete molting. The medicine has high efficiency, low toxicity, is environmentally friendly, and meets people's requirements and development trends for modern pesticides. White powder at room temperature pH=5-9, stable to acid or base catalyzed reaction. Although the present synthetic in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C63/10C07C241/04C07C243/38C07C281/02
CPCC07C51/60C07C241/04C07C281/02C07C63/10C07C243/38
Inventor 张淑芬
Owner SHAANXI QIYUAN TECH DEV
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