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Method for producing fipronil intermediate and by-producing low-carbon ester

A technology of intermediates and low-carbon esters, which is applied in the field of production of low-carbon esters by-product of fipronil intermediates, can solve the problems of production wastewater treatment, waste of resources, etc., and achieve the effect of reducing salt content and CODcr

Inactive Publication Date: 2018-07-03
曾舟华
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] From the production process of the above-mentioned fipronil intermediate, it can be seen that the acetic acid that does not participate in the reaction becomes a part of the wastewater, which not only causes waste of resources, but also brings problems in the treatment of production wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1) Under an ice-salt bath, slowly drop a mixed solution of 30 mL of concentrated sulfuric acid and 30 mL of formic acid into a 250 mL three-necked flask containing 0.12 mol and 8.3 g of sodium nitrite, and keep the reaction temperature at 0-5°C to obtain a thin paste shape. After continuing to stir and react for 15 minutes, add 0.1mol of 2,6-dichloro-4-trifluoromethylaniline and 50mL of 23g formic acid solution to the system dropwise. The reaction solution was cooled to obtain a light brown diazotization solution;

[0016] 2) Keep the diazotization solution below 15°C, add 0.12 mol of methyl 2,3-dicyanopropionate and 50 mL of 16 g formic acid solution dropwise, and continue stirring for 1 hour to obtain a condensate;

[0017] 3) In the condensation liquid, add 140mL methanol, carry out normal pressure or reduced pressure reactive distillation, obtain methyl formate by-product;

[0018] 4) Cool the residual liquid to normal temperature, add 50 mL of water to dilute, ex...

Embodiment 2

[0020] 1) Under the ice-salt bath, slowly drop the mixed solution of 30L concentrated sulfuric acid and 30L glacial acetic acid into a 250L reaction kettle equipped with sodium nitrite 0.12kmol, 8.3kg, and keep the reaction temperature at 0-5°C to obtain dilute paste. After continuing to stir and react for 15 minutes, add 0.1kmol of 2,6-dichloro-4-trifluoromethylaniline and 50L of 23kg of glacial acetic acid solution into the system dropwise. , the reaction solution was cooled to obtain a light brown diazotization solution;

[0021] 2) Keep the diazotization solution below 15°C, add 0.12kmol of methyl 2,3-dicyanopropionate and 50L of 16kg glacial acetic acid solution dropwise, and continue stirring for 1 hour to obtain a condensate;

[0022] 3) Add 140L of methanol to the condensation reaction solution, heat, and carry out rectification under reduced pressure to obtain methyl acetate by-product, add a small amount of 50L of water to distill the residue, extract 3 times with 5...

Embodiment 3

[0025] 1) Under the ice-salt bath, slowly drop the mixed solution of 30L concentrated sulfuric acid and 30L glacial acetic acid into a 250L reaction kettle equipped with sodium nitrite 0.12kmol, 8.3kg, and keep the reaction temperature at 0-5°C to obtain dilute paste. After continuing to stir and react for 15 minutes, add 0.1kmol of 2,6-dichloro-4-trifluoromethylaniline and 50L of 23kg formic acid solution to the system dropwise. The reaction solution was cooled to obtain a light brown diazotization solution;

[0026] 2) Keep the diazotization solution below 15°C, add 0.12kmol of ethyl 2,3-dicyanopropionate and 50L of 18kg glacial acetic acid solution dropwise, and continue stirring for 1 hour to obtain a condensate;

[0027] 3) Add a small amount of water to the condensation reaction solution for dilution, extract 3 times with 50 L of dichloromethane, wash with saturated sodium chloride solution to obtain an organic phase, condensation and extraction of the inorganic phase a...

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Abstract

The invention discloses a method for producing a fipronil intermediate and by-producing low-carbon ester. In the prior art, the organic solvent and the by-product are used as the wastewater so as to cause the waste of resources and the environmental pollution. A purpose of the present invention is to solve the problems in the prior art. The method is characterized in that the existing process acetic acid can be used as the solvent, or formic acid or propionic acid and other low-carbon acids can be used to replace acetic acid so as to be used as the solvent, preferably formic acid is used as the solvent; one selected from methanol, ethanol, propanol and other low-carbon alcohols is added to the condensation reaction solution or the condensation extraction inorganic phase and the washing solution, preferably methanol, heating is performed, and normal pressure or pressure reducing esterification and rectification are performed to obtain the by-product low-carbon ester. According to the present invention, the salt content in the generated wastewater is reduced, the CODcr in the produced wastewater is reduced, and the low-carbon ester product is by-produced.

Description

1. Technical field [0001] The invention belongs to the fields of organic synthesis, resource recovery and environmental protection, and particularly relates to a method for producing fipronil intermediate by-product low-carbon ester. 2. Background technology [0002] Fipronil is a phenylpyrazole insecticide with a wide insecticidal spectrum. It mainly has gastric toxicity to pests, and also has contact killing and certain systemic effects. Its mechanism of action is to hinder insect γ-aminobutyric acid Controlled chloride metabolism, so it has high insecticidal activity against important pests such as aphids, leafhoppers, planthoppers, Lepidoptera larvae, flies and Coleoptera, and has no phytotoxicity to crops. The agent can be applied to the soil or sprayed on the leaves. Applying to the soil can effectively control corn root leaf beetle, wireworm and cutworm. When sprayed on the leaves, it has a high level of control effect on diamondback moth, cabbage butterfly, rice th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/44C07C67/08C07C67/54C07C69/06C07C69/14
CPCC07C67/08C07C67/54C07D231/44C07C69/06C07C69/14
Inventor 曾舟华刘晓晖曾彩红黄春保冉敬文
Owner 曾舟华
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