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Preparation method of 2-hydroxyl-3-trifluoromethylpyridine

A technology of trifluoromethylpyridine and hydroxyl, which is applied in the field of preparation of 2-hydroxy-3-trifluoromethylpyridine, can solve the problems of unreported production and manufacturing methods, and achieve large-scale production, simple operation, and market sufficient effect

Inactive Publication Date: 2018-05-08
SHANDONG HUIMENG BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 2-Hydroxy-3-trifluoromethylpyridine has not been mass-produced in China at present, and the specific production method has not been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Fluorination

[0028] Put 2500g of 2-chloro-3-trifluoromethylpyridine into a 5000ml autoclave at one time, then add 750g of hydrogen fluoride into the autoclave, start stirring, and heat up the reaction. The temperature is 130°C and the pressure does not exceed 80bar. React for 48 hours. After the reaction is over, wash the material with water, then neutralize the pH value to 7 with sodium hydroxide, and then obtain 2-fluoro-3-trifluoromethylpyridine after rectification, with a content of >99%.

[0029] (2) Ammonification

[0030] Add 750g of 2-fluoro-3-trifluoromethylpyridine into the ammoniation kettle, add 700g of water to the ammoniation kettle, then feed 250g of liquid ammonia into the ammoniation kettle, raise the temperature to 130°C, and the pressure is not more than 3.0MPa, and react After 10 hours, the temperature was lowered to 90°C, and the material was discharged into the receiving kettle, and the temperature was lowered to 10°C after receiving, centri...

Embodiment 2

[0035] (1) Fluorination

[0036] Put 2500g of 2-chloro-3-trifluoromethylpyridine into a 5000ml autoclave at one time, then add 750g of hydrogen fluoride into the autoclave, start stirring, and heat up the reaction. The temperature is 210°C and the pressure does not exceed 30bar. React for 48 hours. After the reaction is over, wash the material with water, then neutralize the pH value to 7 with sodium hydroxide, and then obtain 2-fluoro-3-trifluoromethylpyridine after rectification, with a content of >99%.

[0037] (2) Ammonification

[0038] Add 750g of 2-fluoro-3-trifluoromethylpyridine into the ammoniation kettle, add 700g of water to the ammoniation kettle, then feed 250g of liquid ammonia into the ammoniation kettle, raise the temperature to 180°C, and the pressure is not more than 3.0MPa, and the reaction After 10 hours, the temperature was lowered to 90°C, and the material was discharged into the receiving kettle, and the temperature was lowered to 10°C after receiving,...

Embodiment 3

[0043] (1) Fluorination

[0044] Put 2500g of 2-chloro-3-trifluoromethylpyridine into a 5000ml autoclave at one time, then add 750g of hydrogen fluoride into the autoclave, start stirring, and heat up the reaction. The temperature is 170°C and the pressure does not exceed 55bar. React for 48 hours. After the reaction is over, wash the material with water, then neutralize the pH value to 7 with sodium hydroxide, and then obtain 2-fluoro-3-trifluoromethylpyridine after rectification, with a content of >99%.

[0045] (2) Ammonification

[0046] Add 750g of 2-fluoro-3-trifluoromethylpyridine into the ammoniation kettle, add 700g of water to the ammoniation kettle, then pass 250g of liquid ammonia into the ammoniation kettle, raise the temperature to 155°C, and the pressure is not more than 3.0MPa, and react After 10 hours, the temperature was lowered to 90°C, and the material was discharged into the receiving kettle, and the temperature was lowered to 10°C after receiving, centri...

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Abstract

The invention relates to the technical field of chemical synthesis, and particularly discloses a preparation method of 2-hydroxyl-3-trifluoromethylpyridine. According to the preparation method disclosed by the invention, by using the 2-chloro-3-trifluoromethylpyridine as a starting raw material, fluorination is carried out under a certain condition so that 2-fluro-3-trifluoromethylpyridine is prepared; ammonolysis reaction is carried out on the 2-fluro-3-trifluoromethylpyridine so as to prepare 2-amino-3-trifluoromethylpyridine; then diazotization reaction is carried out to obtain the 2-hydroxyl-3-trifluoromethylpyridine. The preparation method disclosed by the invention is reliable in process, raw materials are sufficient and easy to get in the market, the production cost is low, an operation is simple, the yield is high, and scale production is facilitated; at present, a preparation method of the same or other components is never seen at home and abroad.

Description

(1) Technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 2-hydroxy-3-trifluoromethylpyridine. (2) Background technology [0002] 2-Hydroxy-3-trifluoromethylpyridine is a valuable chemical of fluorine-containing pyridine heterocycles, mainly used in pharmaceutical intermediates, organic synthesis, organic solvents, and can also be used in dye production, pesticide production and Spices and more. [0003] Fluorine-containing compounds have the characteristics of high membrane permeability, anti-metabolism stability, affinity with lipid membranes, thermal stability and chemical stability, etc., and have been widely used in pesticides. Fluorine-containing pesticides are very important fluorine-containing fine chemicals. It has the characteristics of high selectivity, high adaptability and broad spectrum, high added value, low dosage, low cost, low toxicity, low residue, and environmental friendliness...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/64
CPCC07D213/64
Inventor 肖才根刘树文
Owner SHANDONG HUIMENG BIO TECH CO LTD
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