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A kind of preparation technology of ethylpyridine 4-amino-3,5-dichloro-6-fluoro-2-oxyacetate

A technology of ethyl oxyacetate pyridine and ethyl chloroacetate, which is applied in the field of fine chemicals, can solve the problems of reduced production costs and environmental treatment costs, unfavorable industrial production, and high production costs, so as to reduce environmental treatment costs and improve raw material utilization The effect of low production rate and production cost

Active Publication Date: 2019-02-01
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims to solve the problem of high production cost and low yield of 4-amino-3,5-dichloro-6-fluoro-2-oxyethylpyridine acetate in the prior art, which is not conducive to industrial production, and provides a A clean method for preparing 4-amino-3,5-dichloro-6-fluoro-2-oxyethyl acetate pyridine, by making raw material 3,5-dichloro-2,4,6-trifluoropyridine In the process of preparing 4-amino-3,5-dichloro-6-fluoro-2-oxyacetic acid ethyl pyridine through amination, hydroxylation and condensation, the by-products and waste liquid generated are processed, and the utilization rate of raw materials It has been improved, the environmental pollution is small, and the production cost and environmental treatment cost are greatly reduced

Method used

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  • A kind of preparation technology of ethylpyridine 4-amino-3,5-dichloro-6-fluoro-2-oxyacetate
  • A kind of preparation technology of ethylpyridine 4-amino-3,5-dichloro-6-fluoro-2-oxyacetate
  • A kind of preparation technology of ethylpyridine 4-amino-3,5-dichloro-6-fluoro-2-oxyacetate

Examples

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Effect test

Embodiment 1

[0051] A preparation process of 4-amino-3,5-dichloro-6-fluoro-2-oxyl ethyl pyridine, characterized in that: comprising the following steps:

[0052] A. Amination

[0053] Add 3,5-dichloro-2,4,6-trifluoropyridine and NMP into the reactor, pass through ammonia gas, after the reaction is complete, filter the reaction solution, and rectify the filtrate to obtain 4-amino-3, 5-dichloro-2,6-difluoropyridine; the waste residue obtained by the filtration is the by-product NH 4 F, the filtrate is a mixture of solvent NMP and 3,5-dichloro-2,4,6-trifluoropyridine. After rectification, NMP and 4-amino-3,5-dichloro-2,6-dichloropyridine are obtained respectively flupyridine;

[0054] B. Hydroxylation

[0055] After adding KOH aqueous solution to the 4-amino-3,5-dichloro-2,6-difluoropyridine obtained in step A, heat to reflux. After the reaction is complete, cool and centrifuge to obtain the mother liquor and solid 4-amino- Potassium 3,5-dichloro-6-fluoropyridin-2-ol;

[0056] C. Mother ...

Embodiment 2

[0062] In this example, on the basis of Example 1, in step A, the amount of ammonia gas introduced is 2.1 times the amount of 3,5-dichloro-2,4,6-trifluoropyridine.

Embodiment 3

[0064] In this example, on the basis of Example 1, in step A, the rectification condition is 80-140°C, and the fraction collected at 122-125°C / 1Kpa is 4-amino-3,5-dichloro-2 ,6-Difluoropyridine.

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Abstract

The invention discloses a preparation process of 4-amino-3, 5-dichloro-6-fluoro-2-ethyl oxy-acetate pyridine and belongs to the technical field of fine chemical engineering. The preparation process includes steps of amination hydroxylation, mother liquid extraction, condensation and byproduct treatment. By fully recycling byproducts and re-extracting waste liquid in the reaction process, raw material utilization rate is increased, product cost and byproduct treatment cost are lowered, and the preparation process is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation process of ethyl 4-amino-3,5-dichloro-6-fluoro-2-oxyacetate pyridine, which belongs to the technical field of fine chemicals. Background technique [0002] Fluroxypyr is a pyridyloxyacetic acid herbicide with systemic transduction effect and typical hormone-type herbicide response. When used post-emergence, sensitive crops show typical hormonal herbicide responses. It has a wide application period on cereal crops, and can be used to control broad-leaved weeds in wheat, barley, corn, grapes, orchards, pastures, forest farms, etc. Amaranth, purslane and other weeds. [0003] 4-Amino-3,5-dichloro-6-fluoro-2-oxyethyl acetate pyridine is the key intermediate for the synthesis of fluroxypyr herbicide. There are many synthetic methods used in the prior art, such as Publication No. It is CN104592103A, an invention patent titled "a synthetic method of fluroxypyr ester". The synthetic method disclosed in this patent is t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 彭舟罗茜李舟王蕾张华皮亚威
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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