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Method for preparing 3, 5, 6-trichloropyridin-2-ol sodium

A technology of trichloropyridine and tetrachloropyridine, which is applied in the field of 3,5,6-trichloropyridin-2-ol sodium, can solve the problems of large material loss, difficulty, and post-treatment of corroded equipment, so as to reduce emissions and improve Utilization rate, damage reduction effect

Active Publication Date: 2012-02-15
JIANGSU JIUJIUJIU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In these two patents, phosphorus oxychloride is used as the chlorination agent in the cyclization step, which corrodes the equipment and is difficult to post-process, resulting in large material loss, which is not conducive to the health of personnel and industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 100.00g of 99.5% trichloroacetyl chloride into a 250ml four-necked flask, add dropwise 19.34g of 99.5% methanol under stirring, drop it in half an hour, then keep it at 60°C for half an hour, distill off excess methanol, and obtain a content of 98 % of methyl trichloroacetate 98.03g, the yield reached 99%.

[0024] Add the above-mentioned methyl trichloroacetate and 0.96g CuCl into a 250ml four-necked flask, stir and raise the temperature to 140°C, add 40.16g of acrylonitrile dropwise, drop it over 3 hours, then raise the temperature to 140°C for 3 hours. Excess acrylonitrile was removed by distillation, and 135.95 g of methyl 2,2,4-trichloro-4-cyanobutyrate with a content of 78% was obtained by suction filtration, with a yield of 85%.

[0025] Add the above methyl 2,2,4-trichloro-4-cyanobutyrate, 252.45g of 99.5% trichloroacetyl chloride and 3.88g of methanol into a 1L autoclave, raise the temperature to 140°C for 8 hours, then cool down and release the pressure ﹝...

Embodiment 2

[0029] Repeat Example 1, but add Cu 2 CuCl was replaced by O to obtain 81.91 g of sodium 3,5,6-trichloropyridin-2-oxide with a content of 78%, and a yield of 53%.

Embodiment 3

[0031] Example 1 was repeated, but the reaction was maintained for 4 hours during cyclization, and 80.37 g of sodium 3,5,6-trichloropyridin-2-olate with a content of 75% was obtained, with a yield of 50%.

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PUM

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Abstract

The invention discloses a method for preparing 3, 5, 6-trichloropyridin-2-ol sodium. The method comprises the steps of esterification reaction, addition reaction, cyclization reaction, hydrolysis reaction and the like. In the method, trichloroacetic chloride is used as the chlorinating agent of the cyclization reaction; and by dropwise adding alcohol, the residual trichloroacetic chloride is converted to trichloroacetate. Therefore, the problem of cyclization material conversion can be solved and the damage of the chlorinating agent with high corrosivity to human body can be reduced. The method is characterized in that trichloroacetate can further be used as the addition raw material, thus the utilization rate of trichloroacetic chloride can be greatly increased, the emission of the phosphorus-containing wastewater can be reduced and the molar yield of sodium alkoxide can reach 68%.

Description

technical field [0001] The invention relates to a method of sodium 3,5,6-trichloropyridin-2-alcohol. Background technique [0002] 3,5,6-trichloropyridin-2-ol sodium is an important intermediate in the synthesis of insecticides chlorpyrifos, chlorpyrifos-methyl and herbicide triclopyr. The synthesis reaction conditions of sodium alkoxide are harsh, the technical difficulty is high, and the production cost is high, which are the main factors affecting the production capacity and cost of downstream products. At present, the more economical and feasible route for industrially synthesizing sodium alkoxide is the trichloroacetyl chloride method. The main disadvantage of this method is that the content and yield of sodium alkoxide are not ideal, the general yield is not more than 65%, and the discharge of "three wastes" is large. [0003] For the above defects, domestic and foreign patents in recent years have proposed a new process for preparing tetraclopyridine and sodium tric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/64
Inventor 周新基
Owner JIANGSU JIUJIUJIU TECH
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