Insecticide indoxacarb intermediate and compounding technology thereof

A technology for indoxacarb and intermediates, which is applied in the preparation of carbon-based compounds, the preparation of organic compounds, and the preparation of carbonyl compounds by condensation, can solve the problems of low insecticidal activity, and achieve improved insecticidal activity, high yield, and optimization. Effects of process parameters

Inactive Publication Date: 2017-09-01
LIANYUNGANG GUOSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides an intermediate of the insecticide indoxacarb and its synthesis process, which has the advantages of directly affecting the enantiomeric excess value and improving the activity of the insecticide, and solves the problem of the existing indoxacarb The problem of low insecticidal activity of intermediates

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment one: a kind of synthetic technique of insecticide indoxacarb intermediate, comprises the following steps:

[0037] S1) Preparation of 3-chloropropionyl chloride: at normal temperature, add 25 parts of hydrochloric acid and 30 parts of sodium chloride to the four-necked bottle, stir, and drop 15 parts of concentrated sulfuric acid into the four-necked bottle through a constant pressure funnel to obtain hydrogen chloride gas, then add 15 parts of acrylic acid in the four-necked bottle, and pass into the hydrogen chloride gas that has been produced, and the temperature is controlled at about 45 degrees, and the light yellow 3-chloropropionic acid solid is obtained, and the yield is 90%. Add the prepared 3-chloropropionic acid solid into the four-necked bottle, heat it to about 50 degrees, then add 6 parts of phosphorus trichloride, raise the temperature to 75 degrees, and precipitate colorless and transparent 3-chloropropionyl chloride through vacuum distillation...

Embodiment 2

[0042] Embodiment two: a kind of synthetic technique of insecticide indoxacarb intermediate, comprises the following steps:

[0043]S1) Preparation of 3-chloropropionyl chloride: at normal temperature, add 30 parts of hydrochloric acid and 35 parts of sodium chloride into the four-necked bottle, stir, and drop 16 parts of concentrated sulfuric acid into the four-necked bottle through a constant pressure funnel to obtain hydrogen chloride gas, then add 17 parts of acrylic acid in the four-necked bottle, and pass into the hydrogen chloride gas that has been produced, and the temperature is controlled at about 45 degrees, and the light yellow 3-chloropropionic acid solid is obtained, and the yield is 92%. Add the prepared 3-chloropropionic acid solid into the four-necked bottle, heat it to about 50 degrees, then add 7 parts of phosphorus trichloride, raise the temperature to 75 degrees, and precipitate colorless and transparent 3-chloropropionyl chloride through vacuum distillatio...

Embodiment 3

[0048] Embodiment three: a kind of synthetic technique of insecticide indoxacarb intermediate comprises the following steps:

[0049] S1) Preparation of 3-chloropropionyl chloride: at normal temperature, add 35 parts of hydrochloric acid and 40 parts of sodium chloride into the four-necked bottle, stir, and drop 18 parts of concentrated sulfuric acid into the four-necked bottle through a constant pressure funnel to obtain hydrogen chloride gas, then add 20 parts of acrylic acid in the four-necked bottle, and pass into the hydrogen chloride gas that has been produced, and the temperature is controlled at about 45 degrees, and the light yellow 3-chloropropionic acid solid is obtained, and the yield is 95%. Add the prepared 3-chloropropionic acid solid to the four-necked bottle, heat it to about 50 degrees, then add 8 parts of phosphorus trichloride, raise the temperature to 75 degrees, and precipitate colorless and transparent 3-chloropropionyl chloride through vacuum distillatio...

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PUM

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Abstract

The invention discloses an insecticide indoxacarb intermediate, which comprises the following raw materials in proportion by weight: acrylic acid: 15-20 parts; chlorobenzene: 40-50 parts; sodium chloride: 30-40 parts; hydrochloric acid : 25‑35 parts; Concentrated sulfuric acid: 70‑85 parts; Phosphorus trichloride: 6‑8 parts; Aluminum trichloride: 23‑30 parts. The insecticide indoxacarb intermediate, its asymmetric selectivity directly affects the enantiomeric excess value of the product during the synthesis process, significantly improving the insecticidal activity, through the S‑(+)‑5‑ Synthesis of Chloro-2,3-Dihydro-2-Hydroxy-1-Oxo-1H-Indene-2-Hydroxy acid methyl ester (indoxacarb intermediate), optimized process parameters and obtained better synthesis The route provides support and theoretical basis for medium-scale scale-up and industrial production, which has important practical significance, and also provides a new S-(+)-5-chloro-2, 3-dihydro-2-hydroxyl- Synthesis process of 1-oxo-1H-indene-2-hydroxy acid methyl ester (indoxacarb intermediate).

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to an intermediate of the pesticide indoxacarb and a synthesis process thereof. Background technique [0002] After nearly a century of development, the world's pesticides have made great progress. However, due to their own defects, traditional pesticides can no longer adapt to the new trend of pesticide development. Therefore, the research direction of pesticides in the world has undergone great changes. , Insecticides, as one of the three major categories of pesticides, have played a huge role in promoting the survival and development of our human beings. Indoxacarb is a typical new type of insecticides, featuring high efficiency and safety, and is environmentally friendly. Pesticides, and S-(+)-5-chloro-2,3-dihydro-2-hydroxyl-1-oxo-1H-indene-2-hydroxy acid methyl ester (indoxacarb intermediate) is the preparation of indazole The key intermediate of indoxacarb, its enantiomeri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/757C07C67/31C07C67/313C07C45/66C07C49/697C07C45/46C07C49/80C07C51/60C07C53/50
CPCC07C69/757C07B2200/07C07C45/46C07C45/66C07C51/60C07C67/31C07C67/313
Inventor 张鑫朱国银周土林徐晨
Owner LIANYUNGANG GUOSHENG CHEM
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