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Synthesis method of 3,5,6-trichloropyridin-2-ol sodium by using 2,3,5,6-tetrachloropyridine as raw material

A technology of tetrachloropyridine and trichloropyridine, which is applied in the field of organic compound synthesis, can solve the problems of increased production cost input, high hazards, and complicated production, and achieve the effects of reducing water costs, cheap prices, and easy availability

Inactive Publication Date: 2016-04-13
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The addition time of this reaction is 24-28 hours, and then it takes 24 hours to filter and desolventize, and then the cyclization can be carried out. The anhydrous acid used in the cyclization is usually hydrogen chloride gas. Relatively large, or some commonly used Lewis acids. Lewis acids are made of sulfuric acid, hydrochloric acid and other acids in a certain proportion. The production is complicated, the price is relatively expensive, and the production cost input is greatly increased.

Method used

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  • Synthesis method of 3,5,6-trichloropyridin-2-ol sodium by using 2,3,5,6-tetrachloropyridine as raw material
  • Synthesis method of 3,5,6-trichloropyridin-2-ol sodium by using 2,3,5,6-tetrachloropyridine as raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A kind of method of using 2,3,5,6-tetrachloropyridine as raw material to synthesize 3,5,6-trichloropyridin-2-alcohol sodium of the present invention comprises the following steps:

[0025] (1) Add 217g of 2,3,5,6-tetrachloropyridine to 868g of water, add 120g of sodium hydroxide, and react at 130°C and 0.35MPa for 3h to obtain 3,5,6-trichloropyridine Pyridin-2-alcohol sodium mixed solution, the temperature of the mixed solution is lowered to 85°C;

[0026] (2) Filter the mixed solution of 3,5,6-trichloropyridin-2-alcohol sodium in step (1) while it is hot, and remove a very small amount of unreacted 2,3,5,6-tetrachloropyridine solid , to obtain a filtrate, the 2,3,5,6-tetrachloropyridine solid obtained by filtering can be recovered as the reaction raw material of step (1) pressurized alkali analysis;

[0027] (3) Cool the primary filtrate of step (2) in an ice-water bath, cool down to 10°C, and precipitate sodium alkoxide crystals; then press filter to obtain white 3,5...

Embodiment 2

[0030] A kind of method of using 2,3,5,6-tetrachloropyridine as raw material to synthesize 3,5,6-trichloropyridin-2-alcohol sodium of the present invention comprises the following steps:

[0031] (1) Add 217g of 2,3,5,6-tetrachloropyridine to 868g of water, add 120g of sodium hydroxide, and react at 140°C and 0.4MPa for 4h to obtain 3,5,6-trichloropyridine Pyridin-2-alcohol sodium mixed solution, the mixed solution is cooled to 90°C;

[0032] (2) Filter the mixed solution of 3,5,6-trichloropyridin-2-alcohol sodium in step (1) while it is hot, and remove a very small amount of unreacted 2,3,5,6-tetrachloropyridine solid , to obtain a filtrate, the 2,3,5,6-tetrachloropyridine solid obtained by filtering can be recovered as the reaction raw material of step (1) pressurized alkali analysis;

[0033] (3) Cool the primary filtrate of step (2) in an ice-water bath, lower the temperature to 5°C, and precipitate sodium alkoxide crystals; then perform pressure filtration to obtain whit...

Embodiment 3

[0036] A kind of method of using 2,3,5,6-tetrachloropyridine as raw material to synthesize 3,5,6-trichloropyridin-2-alcohol sodium of the present invention comprises the following steps:

[0037] (1) Add 217g of 2,3,5,6-tetrachloropyridine to 1000g of water, add 100g of sodium hydroxide, and react at 150°C and 0.4MPa for 3h to obtain 3,5,6-trichloropyridine Pyridin-2-alcohol sodium mixed solution, the mixed solution is cooled to 90°C;

[0038] (2) Filter the mixed solution of 3,5,6-trichloropyridin-2-alcohol sodium in step (1) while it is hot, and remove a very small amount of unreacted 2,3,5,6-tetrachloropyridine solid , to obtain a filtrate, the 2,3,5,6-tetrachloropyridine solid obtained by filtering can be recovered as the reaction raw material of step (1) pressurized alkali analysis;

[0039] (3) Cool the primary filtrate of step (2) in an ice-water bath, cool down to 10°C, and precipitate sodium alkoxide crystals; then press filter to obtain white 3,5,6-trichloropyridin-...

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Abstract

The invention discloses a synthesis method of 3,5,6-trichloropyridin-2-ol sodium by using 2,3,5,6-tetrachloropyridine as a raw material. The method comprises the steps of: (1) mixing 2,3,5,6-tetrachloropyridine with water, adding sodium hydroxide, reacting at high temperature and under high pressure for a period of time, cooling to 80-90 DEG C; (2) filtering 3,5,6-trichloropyridin-2-ol sodium mixed solution while hot to obtain a first filtrate; (3) cooling the first filtrate the in an ice-water bath to 5-10 DEG C, and l precipitating sodium alkoxide crystalline; conducting pressure filtration to obtain a white 3,5,6-trichloropyridin-2-ol sodium crystals and a secondary filtrate. The method uses 2,3,5,6-tetrachloropyridine as the raw material, which is cheap and readily available, to reduce production costs; and compared with the prior art, the method reaches the yield of 95%, has simple process operations, and high yield rate.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and in particular relates to a method for synthesizing sodium 3,5,6-trichloropyridin-2-alcohol by using 2,3,5,6-tetrachloropyridine as a raw material. Background technique [0002] 3,5,6-trichloropyridin-2-alcohol sodium is a key intermediate for the synthesis of chlorpyrifos, the improvement of the quality, cost and yield of chlorpyrifos depends on the 3,5,6-trichloropyridin-2-alcohol sodium synthesis. Some researches have been done on the synthesis process of sodium 3,5,6-trichloropyridin-2-olate at home and abroad. According to the starting materials used, there are mainly two routes: pyridine method and ring method. [0003] The pyridine method can be divided into the pyridine derivative method and the pyridine chlorination method, wherein the pyridine derivative method is a commonly used method in the early stage of triclosan synthesis research, that is, firstly synthesiz...

Claims

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Application Information

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IPC IPC(8): C07D213/64
CPCC07D213/64
Inventor 胡玉兵梁锡臣顾起财先斌王长才杨桂宝李文兵张志宏
Owner ANHUI COSTAR BIOCHEM CO LTD
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