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A kind of preparation method of cyanuric fluoride

A technology of cyanuric fluoride and fluorine reaction, which is applied in the direction of organic chemistry, can solve the problems of strong corrosion of equipment, low product yield, high energy consumption of solvent recovery, etc., and achieve strong corrosion of equipment, high energy consumption, Simple operation effect

Active Publication Date: 2020-01-10
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the existing defects in the existing method for preparing cyanuric cyanuric fluoride, such as strong corrosion of equipment, high energy consumption for solvent recovery, low product yield due to side reactions easily occurring under high temperature conditions, and increased difficulty in waste salt treatment. The purpose of the present invention is to It is to provide a method for preparing cyanuric fluoride with mild reaction conditions, strong selectivity and high yield. The method is low in cost, green and environmentally friendly, and is conducive to industrial production

Method used

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  • A kind of preparation method of cyanuric fluoride
  • A kind of preparation method of cyanuric fluoride
  • A kind of preparation method of cyanuric fluoride

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Experimental program
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Effect test

Embodiment 1

[0026] In a dry reaction vessel, add 1,3,5-trichloro-s-triazine (185g, 1mol) and tetrabutylammonium fluoride (861g, 3.3mol), anhydrous dimethyl sulfoxide (390g, 5.0mol) . The reaction was stirred at 50°C for 6 hours, (TCL followed the reaction). Change the reaction device into a distillation device, distill under reduced pressure, the reduced pressure is 0.012 MPa, collect 124.2 grams of colorless liquid with a boiling point of about 70 ° C, the content of the product measured by GC is 99.2%, and the yield is 92%. Under low temperature conditions, cyanuric fluoride is stored in containers made of polytetrafluoroethylene.

Embodiment 2

[0030] In a dry reaction vessel, add 1,3,5-trichloro-s-triazine (370g, 2mol) and tetrabutylammonium fluoride (1.722kg, 6.6mol), anhydrous dimethyl sulfoxide (780g, 10.0mol ), stirred and reacted at 60°C for 6 hours. (TCL tracking response). The reaction device was changed into a distillation device, vacuum distillation, the reduced pressure was 0.013 MPa, and 257 grams of colorless liquid with a boiling point of about 70° C. was collected. The content of the product measured by GC was 99.0%, and the yield was 95%. Under low temperature conditions, cyanuric fluoride is stored in containers made of polytetrafluoroethylene.

Embodiment 3

[0034] In a dry reaction vessel, add 1,3,5-trichloro-s-triazine (278g, 1.5mol) and tetrabutylammonium fluoride (1.57kg, 6.0mol), anhydrous dimethyl sulfoxide (702g, 9.0 mol), the reaction was stirred at 60°C for 6 hours. (TCL tracking response). The reaction device was changed into a distillation device, vacuum distillation, the reduced pressure was 0.013 MPa, and 188 grams of colorless liquid with a boiling point of about 70° C. was collected. The content of the product measured by GC was 99.0%, and the yield was 93%. Under low temperature conditions, cyanuric fluoride is stored in containers made of polytetrafluoroethylene.

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Abstract

The invention discloses a preparation method of cyanuric fluoride. The method is to carry out fluorination reaction of 1,3,5-trichloro-s-triazine and tetrabutylammonium fluoride to obtain cyanuric fluoride and tetrabutyl ammonium fluoride. Ammonium chloride; this method does not need to use a catalyst, the reaction selectivity is high, the yield can be as high as 95%, and the use of high-risk fluorine reagent hydrogen fluoride or a large amount of metal fluoride and the addition of expensive catalysts are avoided, and the operation is simple and the reaction conditions Temperature, low cost and other advantages, suitable for industrial production.

Description

technical field [0001] The present invention relates to a preparation method of cyanuric fluoride, in particular to a method for efficiently fluorinating 1,3,5-trichloro-s-triazine into cyanuric fluoride by using tetrabutylammonium fluoride as a fluorinating reagent, belonging to Fine chemical industry. Background technique [0002] Cyanuric fluoride, also known as 2,4,6-trifluoro-1,3,5-triazine, cyanuric fluoride, English name: Cyanuricfluoride, 2,4,6-trifluoro-1,3,5-triazine ( TFT). Molecular formula: C 3 f 3 N 3 , the structural formula: [0003] [0004] Trifluorocyanuric fluoride (TFT) is an important fluorinating reagent, which can react with carboxylic acid to generate acyl fluoride (J. Prakt. Chem. 2000, 342, 7, 711-714.). Cyanuric fluoride is an important intermediate of dyes and medicines, and it is a key intermediate for the synthesis of fluoro-s-triazine reactive dyes (EP Patent 1207186 and J Supercrit Fluids 40:477-484.). Because the fluorine atoms wit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/28
CPCC07D251/28
Inventor 严楠余潇兵邱静茹廖维林郭晓红
Owner JIANGXI NORMAL UNIV