Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of N-ethylperfluorohexyl ethanesulfonamide

The technology of fluorohexyl ethyl sulfonamide and ethyl sulfonyl chloride is applied in the field of preparation of N-ethyl perfluorohexyl ethyl sulfonamide, which can solve the problems of strong corrosiveness, excessive waste acid and waste liquid, etc. Sufficient, short reaction time, high purity effect

Inactive Publication Date: 2019-03-15
湖北优世达科技股份有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the direct use of strong oxidizing agents to oxidize perfluoroalkyl iodides, this method is highly corrosive and produces a lot of waste acid and waste liquid.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A preparation method of N-ethylperfluorohexylethylsulfonamide includes the following steps:

[0038] (1) Pass 10.27g of ethylamine gas into 400g of toluene solvent, add 109g of perfluorohexylethylsulfonyl chloride dropwise at a temperature of 75~80℃ for about 1h;

[0039] (2) After the dripping is finished, continue to react and stir for 2h at a temperature of 75~80℃;

[0040] (3) Cool and filter to obtain solids;

[0041] (4) Use 50g of toluene to wash the solids, and toluene is recycled and reused to obtain a residue;

[0042] (5) Use 150g of chloroform to recrystallize the residue at a temperature of 75~80℃;

[0043] (6) Cooling and filtering, the gross weight is 126g, and then drying to obtain 93.2g of N-ethylperfluorohexylethylsulfonamide with a yield of 97.17%.

Embodiment 2

[0045] A preparation method of N-ethylperfluorohexylethylsulfonamide includes the following steps:

[0046] (1) Pass 10.27g of ethylamine gas into 400g of isopropyl ether solvent, add 109g of perfluorohexylethylsulfonyl chloride dropwise at a temperature of 75~80℃, and finish the drop in about 1h;

[0047] (2) After the dripping is finished, continue to react and stir for 2h at a temperature of 75~80℃;

[0048] (3) Cool and filter to obtain solids;

[0049] (4) Use 50 g of isopropyl ether to wash the solids, and the isopropyl ether is recycled and reused to obtain a residue;

[0050] (5) Use 150g of chloroform to recrystallize the residue at a temperature of 75~80℃;

[0051] (6) Cooling and filtering, the gross weight is 128g, and then drying to obtain 94.1g of N-ethylperfluorohexylethylsulfonamide with a yield of 98.1%.

Embodiment 3

[0053] A preparation method of N-ethylperfluorohexylethylsulfonamide includes the following steps:

[0054] (1) Pass 10.27g of ethylamine gas into 400g of toluene solvent, add 100.4g of perfluorohexylethylsulfonyl fluoride dropwise at a temperature of 75~80℃, and finish the drop in about 1h;

[0055] (2) After the dripping is finished, continue to react and stir for 2h at a temperature of 75~80℃;

[0056] (3) Cool and filter to obtain solids;

[0057] (4) Use 50g of toluene to wash the solids, and toluene is recycled and reused to obtain a residue;

[0058] (5) Use 150g of chloroform to recrystallize the residue at a temperature of 75~80℃;

[0059] (6) Cooling and filtering, the gross weight is 126g, and then drying to obtain 90.5g of N-ethylperfluorohexylethylsulfonamide with a yield of 95.17%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method of N-ethylperfluorohexyl ethanesulfonamide. The preparation method comprises the following steps: firstly, dissolving ethylamine gas into a solvent, dropwise adding perfluorohexyl ethanesulfonyl chloride at 50 to 80 DEG C and fully reacting, wherein the molar ratio of the perfluorohexyl ethanesulfonyl chloride to the ethylamine gas is 1 to (1 to 3); secondly, after the dropwise adding is finished, continuously reacting and stirring at 50 to 80 DEG C for 2 to 24 hours; thirdly, cooling and filtering to obtain a solid; fourthly, washing the solid byadopting toluene and recycling the toluene to obtain residues; fifthly, recrystallizing the residues at 75 to 80 DEG C by adopting trichloromethane; and sixthly, cooling, filtering and drying to obtain the N-ethylperfluorohexyl ethanesulfonamide. The preparation method has the advantages of high reaction yield, few by-products and less reaction waste liquid.

Description

Technical field [0001] The invention relates to the technical field of fluorine-containing surfactants and insecticides, in particular to a preparation method of N-ethylperfluorohexylethylsulfonamide. Background technique [0002] Flubendiamide is a new type of phthalamide insecticide, developed by Japan Pesticide Co., Ltd., which can activate the intracellular calcium release channel of the ornidin receptor, resulting in the uncontrolled release of stored calcium ions, which affects almost all scales. Pteran pests all have good activity, and they also have excellent activity on adults and larvae, and have fast action speed and long lasting period without degradation. [0003] In the prior art, the preparation methods of fluorosurfactants that replace PFOA / PFOS are mainly electrolytic fluorination and fluoroalkyl iodide telomerization. Simons et al. described in patent US2519983 that the corresponding hydrocarbon fluoride and acid chloride are used as raw materials, first converte...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/03C07C303/38C07C303/44
CPCC07C303/38C07C303/44C07C311/03
Inventor 刘建国
Owner 湖北优世达科技股份有限公司