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Synthetic method of 5-cholro-8-quinoline oxyacetic acid

A technology of quinolineoxyacetic acid and a synthesis method, which is applied in the field of synthesis of 5-chloro-8-quinolineoxyacetic acid, can solve the problems of environmental pollution in the chlorination step, corroded equipment, low yield and the like, and avoids safety Problems and environmental pollution problems, mild production process conditions, high product yield effects

Inactive Publication Date: 2015-03-04
HARBIN UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of synthetic method of 5-chloro-8-quinolineoxyacetic acid in order to solve the problem of polluting the environment, corroding equipment and low yield in the chlorination step in the existing clofenac-methyl production process

Method used

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  • Synthetic method of 5-cholro-8-quinoline oxyacetic acid
  • Synthetic method of 5-cholro-8-quinoline oxyacetic acid
  • Synthetic method of 5-cholro-8-quinoline oxyacetic acid

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specific Embodiment approach 1

[0020] Specific embodiment 1: A method for synthesizing 5-chloro-8-quinolinoxyacetic acid in this embodiment is completed by the following steps:

[0021] 1. Mix 8-quinolinoxyacetic acid with an aqueous hydrochloric acid solution with a mass percentage of 12%-28% to prepare an 8-quinolinoxyacetic acid electrolyte with a concentration of 5~150g / L; 2. 1. The prepared electrolyte is placed in a single-chamber electrolytic cell, with platinum plates as anode and cathode electrodes, and electrolytic chlorination is carried out for 0.5 to 5 hours under the condition of current intensity of 0.2 to 0.8A; The hydrochloric acid is removed by pressure distillation to obtain crude 5-chloro-8-quinolinoxyacetic acid, and then the crude 5-chloro-8-quinolinoxyacetic acid is refined by recrystallization method to obtain 5-chloro-8-quinoline Pure oxyacetic acid.

specific Embodiment approach 2

[0022] Specific embodiment two: this embodiment is different from specific embodiment one in that the concentration of 8-quinolinoxyacetic acid in step two is 20-120 g / L. Others are the same as the first embodiment.

specific Embodiment approach 3

[0023] Specific embodiment three: This embodiment is different from specific embodiment one or two in that the concentration of 8-quinolinoxyacetic acid in step two is 50-120 g / L. Others are the same as the first or second embodiment.

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Abstract

The invention discloses a synthetic method of 5-cholro-8-quinoline oxyacetic acid, and relates to the technical field of electrochemical organic synthesis. The synthetic method disclosed by the invention is used for solving the problems that the existing cloquitocet-mexyl production process is severe in environmental pollution, poor in selectivity and the like. The operating condition of the method is as follows: in a single-chamber electrolytic tank, platinum sheets are taken as negative and positive electrodes, 8-quinoline oxyacetic acid is taken as a raw material, and aqueous liquor of hydrochloric acid is taken as an electrolyte; 5-cholro-8-quinoline oxyacetic acid can be synthesized with high yield and high selectivity by adjusting the current strength. The method disclosed by the invention mainly has the advantages that chlorine is not directly used in production, so that the safety problem and environmental pollution problem caused by use of chlorine are avoided. In addition, the method provided by the invention is mild in condition of production process, simple to operate, high in product yield, few in byproduct and low in cost, and has greater practical value and social and economical values.

Description

Technical field [0001] The invention relates to a method for synthesizing 5-chloro-8-quinolinoxyacetic acid, which belongs to the technical field of organic electrochemistry. Background technique [0002] The herbicide safener chlorfenapyr can accelerate the detoxification effect of clodinafop-propargyl in grains and has been widely used in the domestic market. 5-Chloro-8-quinolinoxyacetic acid is the main intermediate for the synthesis of chlorotoxyl. 5-chloro-8-quinolinoxy acetic acid is then esterified with 2-heptanol to obtain chlorotoxyl. [0003] The current industrially-used production process of chlorotoluox-methyl is mainly based on 8-hydroxyquinoline as raw material, and chlorine is directly used for chlorination in organic solvents such as chloroform and acetic acid to obtain 5-chloro-8-hydroxyquinoline. This method has poor chlorination selectivity, and has a certain amount of 7-chloro-8-hydroxyquinoline and 5,7-dichloro-8-hydroxyquinoline by-products, which reduces th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D215/28
CPCC25B3/27
Inventor 刘波吕程程由君于艳超
Owner HARBIN UNIV OF SCI & TECH
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