Preparation method of 2-amino-3-chloro-5-(trifluoromethyl) pyridine

A technology of trifluoromethylpyridine and amino, applied in the field of fine chemistry, can solve the problems of harsh production conditions and low yield, and achieve the effects of mild reaction and simple post-processing

Inactive Publication Date: 2010-05-19
NANJING REDSUN BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two methods either have low yields, or use high-temperature and high-pressure equipment, and the production conditions are harsh

Method used

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  • Preparation method of 2-amino-3-chloro-5-(trifluoromethyl) pyridine
  • Preparation method of 2-amino-3-chloro-5-(trifluoromethyl) pyridine

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Embodiment 1

[0014] The preparation of embodiment 1,2-amino-3-chloro-5-trifluoromethylpyridine

[0015] 4.7g 0.12mol NaNH 2 Pulverize and add to 60gDMF, under nitrogen protection, stir and heat to reflux, then add 21.6g 0.1mol 2,3-dichloro-5-trifluoromethylpyridine dropwise to the reaction solution, under nitrogen protection, stir and heat to reflux, and control raw materials After the reaction was complete, the reaction was terminated, filtered, the filtrate was precipitated under reduced pressure, washed with water, and dried to obtain 16.8 g of 2-amino-3-chloro-5-trifluoromethylpyridine with a purity of 98% and a yield of 83.7%.

Embodiment 2

[0016] The preparation of embodiment 2,2-amino-3-chloro-5-trifluoromethylpyridine

[0017] 4.7g 0.12mol NaNH 2 Add 1.5g of 0.025mol ethanolamine into 60g of xylene, nitrogen protection, stir and heat to reflux, then add dropwise 20.0g 0.1mol 2-fluoro-3-chloro-5-trifluoromethylpyridine to the reaction solution, nitrogen Protected, stirred and heated to reflux, the reaction of the central control raw material is complete, the reaction is terminated, filtered, the filtrate is precipitated under reduced pressure, washed with water, and dried to obtain 19.1g of 2-amino-3-chloro-5-trifluoromethylpyridine with a purity of 96% , yield 93.4%.

Embodiment 3

[0018] The preparation of embodiment 3,2-amino-3-chloro-5-trifluoromethylpyridine

[0019] 5.5g 0.14mol NaNH 2 Grinding and adding 6.7g 0.03mol methyl tributyl ammonium chloride to 60g decane, under nitrogen protection, stirred and heated to reflux, then added dropwise 20.0g 0.1mol 2-fluoro-3-chloro-5- Trifluoromethylpyridine, nitrogen protection, stirring and heating to reflux, the reaction of the central control raw material is complete, the reaction is completed, filtered, the filtrate is precipitated under reduced pressure, washed with water, and dried to obtain 2-amino-3-chloro-5-trifluoromethyl Pyridine 19.0g, purity 95%, yield 92.1%.

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Abstract

The invention discloses a preparation method of 2-amino-3-chloro-5-(trifluoromethyl) pyridine, which comprises the steps of: adding sodium amide powder into a solvent which contains or does not contain a phase transfer catalyst, and then, adding 2-halogen-3-chloro-5-(trifluoromethyl) pyridine for reaction at 10-220 DEG C to prepare the 2-amino-3-chloro-5-(trifluoromethyl) pyridine. In the invention, the sodium amide is used as a reagent to react with the 2-halogen-3-chloro-5-(trifluoromethyl) pyridine under the catalytic condition of the phase transfer catalyst at normal pressure to prepare the 2-amino-3-chloro-5-(trifluoromethyl) pyridine. The invention has moderate reaction and simple post treatment.

Description

technical field [0001] The invention belongs to the field of fine chemistry, and in particular relates to a synthesis method of 2-amino-3-chloro-5-trifluoromethylpyridine. Background technique [0002] Fluazinam is a protective aniline fungicide developed by Ishihara Sangyo Co., Ltd. in Japan. It has a broad bactericidal spectrum and long-lasting effect. body. EP0031218 discloses its synthesis method, using ammonia water as a reagent, reacting for 24 hours at 125°C and 2 atmospheres, with a yield of 25%. CN101081833A improves the reaction of EP0031218, uses liquid ammonia as a reagent, and reacts at a high temperature of 130° C. and a high pressure of 3.5 MPa for 8 hours, with a yield of 90%. These two methods either have low yields, or use high-temperature and high-pressure equipment, and the production conditions are harsh. Contents of the invention [0003] The purpose of the present invention is to overcome the above problems and provide a method for preparing 2-ami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/73
Inventor 王文魁陶兴标杨玉林顾福海唐旺全
Owner NANJING REDSUN BIOCHEM CO LTD
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