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Production method of high-efficiency herbicide furazone

A production method, the technology of furazone, which is applied in the production field of the high-efficiency herbicide furazone, can solve the problems of hidden dangers in production safety, inapplicability to industrial production, and difficult operation, and achieve low requirements for reaction purification conditions, which are conducive to wide application, The effect of not being easy to discharge waste acid

Active Publication Date: 2018-07-27
JIANGSU MINGCHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This compound relates to a synthetic method, the method for synthesizing furazone introduced in US Patent No. 4,568,376. All the synthetic processes of this method use ether extraction, which has a large production safety hazard.
The three-step reaction uses different solvents to participate in the reaction. It is difficult to recover and apply the solvent, and it is easy to produce waste acid to discharge and pollute the environment. The process steps are complicated and difficult to operate.
In addition, the reaction purification process is complicated and the reaction yield is low
[0005] To sum up, the traditional synthetic method has production safety hazards and complex process steps, and the reaction yield is low, which is not suitable for industrial production. Therefore, optimizing and improving the above-mentioned traditional process is of great significance to the promotion and application of furazone

Method used

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  • Production method of high-efficiency herbicide furazone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The first step: add 100L of methanol solvent into the reactor, and dissolve 58.4Kg of sodium methoxide in the above-mentioned solvent, slowly add 100Kg of m-trifluoromethylphenylacetonitrile and 115Kg of ethyl phenylacetate mixed solution into it under full stirring, and add the After completion, the reaction was stirred at 25° C. for 16 hours, 250 L of water was added to the mixed liquid, the pH was adjusted to 1 with hydrochloric acid, and then extracted with dichloroethane and concentrated to dryness to obtain intermediate product A.

[0024] The second step: the above-mentioned intermediate product A was dissolved in 200L of methanol, and then 82.1Kg of liquid bromine was slowly added to the above-mentioned solution and stirred at room temperature for 13 hours. After the reaction, sodium sulfite was added to react the excess bromine. Add 200L of water to the mixture, and then extract it three times with dichloroethane to obtain the dichloroethane extract containing t...

Embodiment 2

[0027] The first step: add 100L of methanol solvent into the reactor, and dissolve 73.5Kg of sodium ethoxide in the above-mentioned solvent, and slowly add 100Kg of m-trifluoromethylphenylacetonitrile and 105Kg of ethyl phenylacetate mixture to it under full stirring, and add the After completion, the reaction was stirred at 25° C. for 18 hours, 250 L of water was added to the mixture, the pH was adjusted to 3 with hydrochloric acid, and then extracted with dichloroethane and concentrated to dryness to obtain intermediate product A.

[0028] The second step: the above-mentioned intermediate product A was dissolved in 200L of methanol, and then 80.8Kg of liquid bromine was slowly added to the above-mentioned solution and stirred at room temperature for 13 hours. After the reaction, sodium sulfite was added to react excess bromine. Add 200L of water to the mixture, and then extract it three times with dichloroethane to obtain the dichloroethane extract containing the intermediate...

Embodiment 3

[0031] The first step: Add 100L of methanol solvent into the reactor, and dissolve 93.4Kg of sodium tert-butoxide in the above solvent, and slowly add 100Kg of m-trifluoromethyl phenylacetonitrile and 106Kg of ethyl phenylacetate mixture into it under full stirring , after the addition, stirred and reacted at 25° C. for 15 hours, added 250 L of water to the mixture, adjusted the pH to 3 with hydrochloric acid, extracted with dichloroethane, concentrated to dryness to obtain intermediate product A.

[0032] The second step: the above intermediate product A was dissolved in methanol 200L methanol, then 81.6Kg liquid bromine was slowly added to the above solution and stirred at room temperature for 13 hours, after the reaction was completed, sodium sulfite was added to react excess bromine. Add 200L of water to the mixture, and then extract it three times with dichloroethane to obtain the dichloroethane extract containing the intermediate product B, and put this solution directly ...

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Abstract

The invention discloses a production method of high-efficiency herbicide flurtamone. The production method comprises that a desired product flurtamone is prepared from trifluoromethyl phenylacetonitrile and ethyl phenylacetate as main raw materials through Claisen condensation, cyclization in an acid solvent and methylation. The production method has high safety, low requirements on reaction purifying conditions and product separation easiness, does not easily discharge an acid solution, realizes recovery and recycle of a solvent and has a high production yield. The production method is suitable for flurtamone industrial production and is conducive to wide application of high-efficiency herbicide flurtamone.

Description

technical field [0001] The invention relates to the technical field of pesticide organic synthesis, in particular to a production method of the high-efficiency herbicide furazone. Background technique [0002] Pesticides play a very important role in controlling pests and diseases and increasing crop yields, and the development of modern agriculture is largely accompanied by the development of these pesticides [Ridgway, R.L.; Tinney, J.C.; MacGregor, J.T. et al. Pesticide use in agriculture. Environ. Health. Persp. 1978, 27, 103-108.]. Pesticides include herbicides, insecticides, and fungicides, among which herbicides occupy the largest market. With the continuous development and progress of agricultural technology, the demand for herbicides will also increase, and herbicides will be the development direction of pesticides and the focus of the development of the pesticide industry. [0003] Flurtamone is a kind of herbicide with superior performance. Futrione belongs to p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/66
CPCC07D307/66
Inventor 李小明王超金璐怡
Owner JIANGSU MINGCHEM CORP
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