Synthesis method of 6-fluorosalicylic acid

A synthetic method, the technology of fluorosalicylic acid, applied in the field of preparation of fine chemical compounds, can solve the problems of low yield, increased cost, complicated production, etc., and achieve the effect of simple post-processing

Inactive Publication Date: 2017-01-18
YANGZHOU TIANCHEN FINE CHEM
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

This method needs to be completed in two steps, which complicates the production, lowers the yield and increases the cost

Method used

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Experimental program
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Effect test

Embodiment Construction

[0014] Add 139g 2,6-difluorobenzonitrile, 120g sodium hydroxide and 180g water to the autoclave (the molar ratio of the three is: 1:3:10), heat to 150°C, react for 10 hours, and control the pressure to 0.25 MPa.

[0015] After the reaction was completed, it was cooled, the reaction solution was poured into a beaker, and the pH value was adjusted to 1 with a 10% sulfuric acid aqueous solution, and a slightly yellowish solid was precipitated. After suction filtration, the solid phase was washed with cold water, dried, and then recrystallized with a mixed solution of 300 ml of ethanol and water with a volume ratio of 2:1 to obtain 168.2 g of white crystalline 6-fluorosalicylic acid.

[0016] The yield of 6-fluorosalicylic acid: 85%.

[0017] The purity of 6-fluorosalicylic acid is: 98.5%.

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Abstract

The invention discloses a synthesis method of 6-fluorosalicylic acid, and belongs to the field of preparation of fine chemical compounds. The method includes the steps of mixing 2,6-difluorobenzonitrile, sodium hydroxide and water for reaction under the pressure of 0.25 MPa at the temperature of 150 DEG C, cooling and then adjusting the pH value of reaction liquid through acid liquor, taking out separated solid, washing and drying the solid, dissolving the solid in solvent for recrystallization, and obtaining 6-fluorosalicylic acid. The method is characterized in that the mixing molar ratio of 2,6-difluorobenzonitrile to sodium hydroxide to water is 1:3:10; the acid liquor for adjusting the pH value of the reaction liquid is a sulfuric acid aqueous solution and is used for adjusting the pH value to be 1; the solvent for recrystallization is an ethyl alcohol and water mixed solution. The method is low in production cost and high in yield.

Description

technical field [0001] The invention belongs to the field of preparation of fine chemical compounds. Background technique [0002] At present, there are few introductions and synthetic methods of 6-fluorosalicylic acid at home and abroad. According to the properties and characteristics of other halides of salicylic acid, it can be thought that 6-fluorosalicylic acid has great application in medicines and pesticides. For example, 5-fluorosalicylic acid is an important fluorine-containing drug intermediate. Ankenbauer et al. constructed a synthetic route of salicylic acid synthesis blocking mutant Sal-IA602, 5-fluorosalicylic acid Fig. 1 Synthetic route of 5 -Fluoro-2-chlorobenzonitrile found that only 5-fluorosalicylic acid, etc. can be used in the biosynthesis of pyochelin analogs to generate corresponding microbial drugs, and salicylic acid halides have such great importance in this regard, so it is necessary to Further research and development and breakthroughs. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/08C07C51/43C07C65/10
CPCC07C51/08C07C51/43C07C65/10
Inventor 陈国云王晨潘明生沈忠诚缪有昌刘润兴蔡磊张小凤罗瑞
Owner YANGZHOU TIANCHEN FINE CHEM
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