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Production method of 3,5,6-trichloro pyridine-2-phenolate

A production method, the technology of triclopyridine, applied in the direction of organic chemistry, etc., can solve the problems of low reaction yield, many types of solvents, and easy pollution of the environment, and achieve the effects of high yield, saving raw materials, and easy access to raw materials

Inactive Publication Date: 2004-07-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses many kinds of solvents, complex operation and low reaction yield
The Brazilian patent (BR8703983) uses highly toxic nitrobenzene as a solvent, which is easy to pollute the environment

Method used

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  • Production method of 3,5,6-trichloro pyridine-2-phenolate

Examples

Experimental program
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Effect test

Embodiment 1

[0012] In a 3000L enamel glass reaction kettle, add 1500L p-chlorotoluene, 8.9Kg cuprous chloride, 546Kg trichloroacetyl chloride and 175Kg acrylonitrile in sequence, gradually raise the temperature to 140°C, after 4 hours of reaction, cool down to 40°C, slowly Add 840Kg of 30% sodium hydroxide solution dropwise, then cool, filter and dry to obtain sodium 3,5,6-trichloropyridin-2-ol. The total yield is 63.2%.

Embodiment 2

[0014] In a 3000L enamel glass reaction kettle, add 1500L xylene, 11.4Kg cuprous iodide, 546Kg trichloroacetyl chloride and 191Kg acrylonitrile in sequence, gradually raise the temperature to 135°C, and after 5 hours of reaction, cool the reaction solution to 40°C , slowly add 840Kg30% sodium hydroxide solution dropwise, then cool, filter and dry to obtain 3,5,6-trichloropyridine-2-phenol sodium. The total yield is 62.5%.

Embodiment 3

[0016] In a 3000L enamel glass reaction kettle, add 1500L o-dichlorobenzene, 5.9Kg cuprous chloride, 546Kg trichloroacetyl chloride and 175Kg acrylonitrile in sequence, gradually raise the temperature to 150°C, react for 3 hours, and cool the reaction solution to At 50°C, slowly add an aqueous solution of sodium carbonate dropwise until the pH value of the reaction liquid reaches above 10, then cool, filter and dry to obtain sodium 3,5,6-trichloropyridin-2-ol. The total yield is 63.0%.

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Abstract

A process for preparing 3,5,6-trichloropyridine-2-phenoxide from trichloroacetyl chloride and acrylonitrile includes addition and cyclizing reactions under existance of solvent and catalyst, and aromatizing and neutralizing in alkaline condition. Its advantages are simple process and high output rate.

Description

technical field [0001] The present invention relates to a new process for the production of 3,5,6-trichloropyridine-2-phenol salts. The method is suitable for the occasion of producing 3,5,6-trichloropyridine-2-phenol salt with trichloroacetyl chloride and acrylonitrile as main raw materials. Background technique [0002] 3,5,6-Trichloropyridine-2-phenol salt is an essential intermediate of the high-efficiency, safe, and broad-spectrum insecticide and acaricide chlorpyrifos and the high-efficiency, low-toxicity, and broad-spectrum herbicide triclopyr. Chlorpyrifos can effectively control a variety of pests on crops such as rice, wheat, corn, cotton, fruit trees, vegetables, tea and flowers, as well as underground pests and livestock ectoparasites. It is the first choice to replace highly toxic pesticides. Triclopyr is a systemic herbicide, which is used to control annual and perennial weeds in rice, wheat, rubber plantations and pastures, and has broad application prospects...

Claims

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Application Information

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IPC IPC(8): C07D213/61
Inventor 徐振元许丹倩戴金贵
Owner ZHEJIANG UNIV OF TECH
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