Fluopyram and synthesis method thereof

A technology of fluopyram and its synthesis method, which is applied in the synthesis and application fields of fine chemical products, can solve the problems of low content and yield of fluopyram, high production cost of fluopyram, and poor use effect, etc. Achieve the effect of easy operation and implementation, avoid loss and high utilization rate of raw materials

Active Publication Date: 2018-11-16
陕西恒润化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing fluopyram synthesis process, waste water, waste gas and solid waste will be produced, and the content and yield of fluopyram are all low, the yield is generally about 44%, resulting in the production of fluopyram The cost is high, and its impurity content is high, and the use effect is not good

Method used

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  • Fluopyram and synthesis method thereof
  • Fluopyram and synthesis method thereof
  • Fluopyram and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] A synthetic method for fluopyram, comprising the following steps:

[0049] Step 1, add 96g of o-trifluoromethylbenzoic acid and 200g of thionyl chloride to a 500mL three-necked flask, start stirring at a speed of 95 rpm, heat up to 79°C and reflux for 6 hours, then in a vacuum of -0.085MPa, 55°C negative pressure recovery of thionyl chloride for 1.5 hours to obtain o-trifluoromethylbenzoyl chloride, hydrogen chloride and sulfur dioxide gas; the specific chlorination process is shown in formula (1):

[0050]

[0051] Step 2, add 360g ammoniacal liquor in the there-necked bottle of 500mL, start to stir with rotating speed as 95 revs / min, add o-trifluoromethylbenzoyl chloride dropwise while stirring in ammoniacal liquor, o-trifluoromethylbenzoyl chloride is at 20 Add dropwise in 30 minutes under the condition of ℃, continue to stir for 1 hour, then filter under the condition of vacuum degree of -0.085MPa for 10 minutes, and dry at 80 ℃ for 3 hours to obtain 90g of o-tri...

Embodiment 2

[0063] A synthetic method for fluopyram, comprising the following steps:

[0064] Step 1, add 90g of o-trifluoromethylbenzoic acid and 180g of thionyl chloride to a 500mL three-necked flask, start stirring at a speed of 95 rpm, heat up to 79°C and reflux for 5.5 hours, then in a vacuum of -0.090MPa, 45°C under negative pressure to recover thionyl chloride for 1.7 hours to obtain o-trifluoromethylbenzoyl chloride, hydrogen chloride and sulfur dioxide gas.

[0065] Step 2, add 340g ammoniacal liquor in the there-necked bottle of 500mL, start to stir with rotating speed at 95 rpm, add o-trifluoromethylbenzoyl chloride dropwise while stirring in ammoniacal liquor, o-trifluoromethylbenzoyl chloride is at 15 Add dropwise in 36 minutes under the condition of ℃, continue to stir for 1.1 hours, then filter under the condition of vacuum degree of -0.087MPa for 15 minutes, and dry at 75℃ for 3.2 hours to obtain o-trifluoromethylbenzamide white Solid, 93.2% yield from the first two steps...

Embodiment 3

[0072] A synthetic method for fluopyram, comprising the following steps:

[0073] Step 1, add 102g of o-trifluoromethylbenzoic acid and 220g of thionyl chloride to a 500mL three-necked flask, start stirring at a speed of 95 rpm, heat up to 79°C and reflux for 6.5 hours, then in a vacuum of -0.085MPa, 55°C under negative pressure to recover thionyl chloride for 1.3 hours to obtain o-trifluoromethylbenzoyl chloride, hydrogen chloride and sulfur dioxide gas.

[0074] Step 2, add 360g ammoniacal liquor in the there-necked bottle of 500mL, start to stir with rotating speed as 95 revs / min, add o-trifluoromethylbenzoyl chloride dropwise while stirring in ammoniacal liquor, o-trifluoromethylbenzoyl chloride is at 15 Add dropwise in 30 minutes under the condition of ℃, continue to stir for 1.2 hours, then filter under the condition of vacuum degree of -0.090MPa for 10 minutes, and dry at 85℃ for 2.8 hours to obtain o-trifluoromethylbenzamide white Solid, 93.1% yield from the first two...

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Abstract

The invention discloses fluopyram and a synthesis method thereof. The fluopyram comprises the following raw materials: trifluoromethylbenzoic acid, thionyl chloride, ammonia water, water, potassium carbonate, paraformaldehyde, formamide, acetic anhydride, 5-trifluoromethyl-2-dimethyl malonate--3-chloropyridine, sodium chloride and hydrochloric acid. The content of fluopyram obtained in the invention is 98% or more, and the total yield of fluopyram is 63% or more. The synthesis method of the invention does not use cyano groups with high activity, and the yield of aminolysis can reach 93%; the raw materials are simple to treat and high in utilization rate; waste gas, waste water and industrial residues are not produced; and the synthesis method is simple in process and easy to operate and implement.

Description

technical field [0001] The invention relates to the technical field of synthesis and application of fine chemical products, in particular to fluopyram and a synthesis method thereof. Background technique [0002] Fluopyram is not only a new generation of excellent nematocide, but also a broad-spectrum fungicide, seed treatment agent, storage and preservation agent for agricultural products, etc., with multi-functionality. It inhibits mitochondrial respiration by blocking electron transfer from succinate dehydrogenase in the respiratory chain. The purpose of controlling pathogenic bacteria is achieved by inhibiting several stages in the growth cycle of pathogenic bacteria. It is mainly used to prevent and control diseases caused by Ascomycetes on broad-leaved crops. [0003] In the existing fluopyram synthesis process, waste water, waste gas and solid waste will be produced, and the content and yield of fluopyram are all low, the yield is generally about 44%, resulting in th...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 樊明李仓珍谌敦国
Owner 陕西恒润化学工业有限公司
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