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Method for producing chlorfenapyr intermediate pyrrole by replacing acetonitrile with solvent DMF

An intermediate, chlorfenapyr technology, applied in the field of chlorfenapyr production, can solve problems such as ineffective improvement, low yield of intermediate products, increased production costs, etc., so as to reduce the production burden of enterprises, reduce energy consumption for recycling, Effect of production cost reduction

Pending Publication Date: 2021-04-06
李通
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] (1) Overcome the problem that the reaction temperature cannot be raised to 80°C due to the limitation of acetonitrile's own characteristics, resulting in incomplete and incomplete conversion in the later stage of the reaction, and the yield of intermediate products is always lower than 85%, and cannot be effectively improved
[0012] (2) To overcome the problems of large recovery loss of acetonitrile in the later recovery process, resulting in waste of resources and increased production costs

Method used

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  • Method for producing chlorfenapyr intermediate pyrrole by replacing acetonitrile with solvent DMF
  • Method for producing chlorfenapyr intermediate pyrrole by replacing acetonitrile with solvent DMF

Examples

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Embodiment 1

[0049] A kind of method that solvent DMF replaces acetonitrile to produce chlorfenapyr intermediate pyrrole, adopts DMF to replace acetonitrile as solvent.

[0050] The method that described solvent DMF replaces acetonitrile to produce chlorfenapyr intermediate pyrrole, comprises the following steps:

[0051] (1) After the lactonization reaction, remove acetonitrile; then add benzene-water mixture, heat up to 40°C, and extract to obtain 4-(p-chlorophenyl)-2-trifluoromethyl-3-oxazoline- 5-ketone, content > 90%; then add 2 times the weight of DMF, stir at 85RPM for 30 minutes, and fully mix to obtain a mixed material.

[0052] During the process of removing acetonitrile, the vacuum degree is maintained at -0.1 MPa, and the temperature is slowly raised to 65° C. at a rate of 0.1-1° C. / min.

[0053] The acetonitrile is removed, and when the temperature is raised to 65° C., a sample is taken to detect the acetonitrile content, and the following treatment is carried out according t...

Embodiment 2

[0072] A kind of method that solvent DMF replaces acetonitrile to produce chlorfenapyr intermediate pyrrole, adopts DMF to replace acetonitrile as solvent.

[0073] The method that described solvent DMF replaces acetonitrile to produce chlorfenapyr intermediate pyrrole, comprises the following steps:

[0074] (1) After the lactonization reaction, remove acetonitrile; then add benzene-water mixture, heat up to 40°C, and extract to obtain 4-(p-chlorophenyl)-2-trifluoromethyl-3-oxazoline- 5-ketone, content > 90%; then add 1.8 times the weight of DMF, stir at 75RPM for 20 minutes, and fully mix to obtain a mixed material.

[0075] During the process of removing acetonitrile, the vacuum degree was kept at -0.1 MPa, and the temperature was slowly raised to 65° C. at a rate of 1° C. / min.

[0076] The acetonitrile is removed, and when the temperature is raised to 65° C., a sample is taken to detect the acetonitrile content, and the following treatment is carried out according to the ...

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Abstract

The invention provides a method for producing chlorfenapyr intermediate pyrrole by replacing acetonitrile with a solvent DMF. The solvent DMF is used for replacing acetonitrile. The method for producing the chlorfenapyr intermediate pyrrole by replacing acetonitrile with the solvent DMF comprises the following steps: extraction replacement, heat preservation reaction and condensation desolvation. The method has the beneficial effects that the reaction temperature of the pyrrolation cyclization reaction for preparing the intermediate is increased to 80 DEG C, the yield is increased to 90% or above in a breakthrough manner, the consumed solvent amount is reduced by more than 30%, the production cost is reduced by about 86%, the production cost is greatly reduced, and the production burden of enterprises is reduced.

Description

technical field [0001] The invention relates to the field of chlorfenapyr production, in particular to a method in which the solvent DMF replaces acetonitrile to produce chlorfenapyr intermediate pyrrole. Background technique [0002] Chlorfenapyr, English name Chlorfenapyr, Chinese common name Chlorfenapyr. It is a new type of heterocyclic insecticide, acaricide and nematicide successfully developed by American Cyanamid Company. With the promulgation of the national highly toxic pesticide substitution policy and the improvement of people's awareness of environmental protection, as a representative of the recommended pesticide varieties for pest control of pollution-free agricultural products, chlorfenapyr with low toxicity and high efficiency has also attracted more and more attention. [0003] Chlorfenapyr, an arylpyrrole compound, is non-toxic to insects itself. After insects feed or contact with chlorfenapyr, in the insect body, chlorfenapyr is converted into a specifi...

Claims

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Application Information

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IPC IPC(8): C07D207/34
CPCC07D207/34
Inventor 李通
Owner 李通
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