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New synthesis technique of 3,5,6-trichloropyridyl-2-sodium alkoxide

A technology of trichloropyridine and synthesis technology, applied in the new synthesis technology field, can solve the problems of many by-products in the one-step addition and cyclization method, being unsuitable for industrial large-scale production, difficult to large-scale production, etc. The effect of improved performance and yield, and low cost of production equipment

Inactive Publication Date: 2014-12-03
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acrylic acid method first needs to prepare acryloyl chloride. There are many synthesis steps and a long route. The reaction process also needs to add expensive catalysts such as organophosphorus and organotin, which is not suitable for large-scale industrial production.
The phenyl trichloroacetate method requires a large amount of valuable solvent sulfolane, and the by-products are not easy to recover, the yield is low, and it is not easy to produce on a large scale
[0004] The technical problem to be solved by this invention is to provide a kind of trichloroacetyl chloride one-step method to prepare 3,5,6-trichloropyridin-2-ol sodium salt, This method not only has low production equipment cost, simple operation and short process, but also effectively solves the problem of many by-products and difficult separation in the one-step addition and cyclization process, and the selectivity and yield of triclopyridinate sodium are effectively improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 3000L enamel glass reactor, add 546Kg trichloroacetyl chloride, 190.8kg acrylonitrile, 1638kg chlorinated benzene, 2.73Kg cuprous chloride, 5.46Kg copper powder, and control the reflux reaction temperature at 100°C-125°C. After 30 hours, after the addition reaction, cool down to 60°C, add 2.73g of trialkylamine, and react for 4 hours. After the reaction, filter out the catalyst, and remove 3 / 4 of the filtrate at -0.8~0.9MP. Then the remaining liquid is discharged into the crystallization tank, the pyridone solution is cooled and crystallized, separated and dried to obtain pyridone. Mix 1 part of pyridone and 3 parts of water into the alkali analysis kettle, add dropwise 20% NaOH solution, control the reaction temperature not to exceed 50°C, adjust the pH to 11, keep it at 40°C for 2 hours, and then filter to obtain trichloropyridine Sodium alkoxide, the yield is 78%.

Embodiment 2

[0027] In a 3000L enamel glass reaction kettle, add 546Kg trichloroacetyl chloride, 190.8kg acrylonitrile, 1638kg chlorinated benzene, 2.73Kg cuprous chloride, 5.46Kg copper powder, and control the reflux reaction temperature at 100°C-125°C. After 30 hours, after the addition reaction, cool down to 60°C, add 2.73g of pyridine, and react for 4 hours. After the reaction, filter out the catalyst, and remove 3 / 4 of the filtrate at -0.8~0.9MP. Then the remaining liquid is discharged into the crystallization tank, the pyridone solution is cooled and crystallized, separated and dried to obtain pyridone. Mix 1 part of pyridone and 3 parts of water into the alkali analysis kettle, add dropwise 20% NaOH solution, control the reaction temperature not to exceed 50°C, adjust the pH to 11, keep it at 40°C for 2 hours, and then filter to obtain trichloropyridine Sodium alkoxide, the yield is 75%.

Embodiment 3

[0029] In a 3000L enamel glass reaction kettle, add 546Kg trichloroacetyl chloride, 190.8kg acrylonitrile, 1638kg chlorinated benzene, 2.73Kg cuprous chloride, 5.46Kg copper powder, and control the reflux reaction temperature at 100°C-125°C. After 30 hours, after the addition reaction, cool down to 60°C, add 2.73g of lutidine, and react for 4 hours. After the reaction, filter off the catalyst, and remove 3 / 4 of the filtrate at -0.8~0.9MP. Then the remaining liquid is discharged into the crystallization tank, the pyridone solution is cooled and crystallized, separated and dried to obtain pyridone. Mix 1 part of pyridone and 3 parts of water into the alkali analysis kettle, add dropwise 20% NaOH solution, control the reaction temperature not to exceed 50°C, adjust the pH to 11, keep it at 40°C for 2 hours, and then filter to obtain trichloropyridine Sodium alkoxide, the yield is 81%.

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Abstract

The invention provides a new synthesis technique of 3,5,6-trichloropyridyl-2-sodium alkoxide, which comprises the following steps: by using trichloro-acetic chloride and acrylonitrile as raw materials, carrying out one-step addition cyclization under the actions of a specific solvent and a specific catalyst to obtain 3,3,5,6-tetrachloro-4,4-dihydropyridyl-2-one, desolventizing, crystallizing, and carrying out alkali resolution to obtain the 3,5,6-trichloropyridyl-2-sodium alkoxide. The technique has the characteristics of lower cost of production equipment, simple production equipment, short process, higher reaction yield and the like, and is simple to operate and suitable for industrial production.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a new synthesis process of sodium 3,5,6-trichloropyridin-2-alcohol. Background technique [0002] Sodium 3,5,6-trichloropyridin-2-ol, formula C 5 HONCl 3 Na, molecular weight 220.5, pure product is white solid, is an important chemical raw material, mainly used as the main intermediate in the synthesis of low-toxicity, broad-spectrum, low-residue organic insecticides and acaricides such as chlorpyrifos and chlorpyrifos-methyl. [0003] The synthetic methods of 3,5,6-trichloropyridin-2-alcohol sodium are divided according to the starting materials used, mainly including pyridine method and ring method. The pyridine method includes a pyridine liquid phase chlorination method and a pyridine gas phase chlorination method. The pyridine liquid phase chlorination method has a low yield of sodium alkoxide, consumes a large amount of solvent, and is not suitable for large-scale...

Claims

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Application Information

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IPC IPC(8): C07D213/64
CPCC07D213/64
Inventor 方红新张涛王晓亭
Owner ANHUI COSTAR BIOCHEM CO LTD
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