Synthesis method of N, N-dimethyl trifluoromethanesulfonamide

Abstract

The invention discloses a synthesis method of N, N-dimethyl trifluoromethanesulfonamide, and relates to the technical field of battery electrolyte additives, and the synthesis method comprises the following steps: taking trifluoromethanesulfonyl fluoride and dimethylamine, and carrying out amidation reaction under the condition of 0.1-0.5 MPa to obtain the N, N-dimethyl trifluoromethanesulfonamide. The preparation method comprises the following steps: taking trifluoromethanesulfonyl fluoride and dimethylamine as raw materials, and directly carrying out amidation reaction; the reaction process is simple, raw materials used in the reaction are easy to obtain, the reaction process is milder and safer compared with the prior art, the product yield and product purity maximization in the production process are guaranteed through control over reaction conditions in all stages, the product yield is further increased by reasonably controlling the use amount of the reaction raw materials and the reaction process, the yield reaches 88.29% or above, and the purity reaches 99.5% or above.

Description

technical field

[0001] The invention relates to the technical field of battery electrolyte additives, in particular to a synthesis method of N,N-dimethyltrifluoromethanesulfonamide. Background technique

[0002] Lithium-ion batteries are currently the most common electrical energy storage devices. Compared with traditional batteries, they have higher storage capacity and more stable performance. The key factors affecting the performance of lithium-ion batteries lie in the performance of organic electrolytes. In battery production, an electrolyte additive containing N,N-dimethyltrifluoromethanesulfonamide is added to the electrolyte to increase the concentration of hydrogen ions in the electrolyte and reduce the loss in the process of electric energy conversion.

[0003] In the prior art, the preparation process of N,N-dimethyltrifluoromethanesulfonamide mainly generates N,N-dimethyltrifluoromethanesulfonamide through the reaction of trifluoromethanesulfonamide and methyl hal...

Examples

Embodiment 1

[0021] The synthetic method of N,N-dimethyltrifluoromethanesulfonamide, its synthetic steps are as follows:

[0022] Take 16.91g (0.15mol) of 40wt% dimethylamine aqueous solution and add it to the autoclave, cool down to 5°C, slowly add 15.2g (0.1mol) trifluoromethanesulfonyl fluoride dropwise, after the dropwise addition, add 8.1g (0.08mol) triethylamine, then increase the pressure to 0.5MPa, maintain 0.5MPa and raise the temperature to 20°C for amidation reaction for 20h, after the amidation reaction is completed, concentrate, and then use ether as the eluent to go through column chromatography Purify, collect, concentrate the eluent, and concentrate under reduced pressure to obtain 15.89 g of N,N-dimethyltrifluoromethanesulfonamide with a yield of 89.70% and a purity of 99.5%. The specific chemical reaction formula is as follows:

[0023]

Embodiment 2

[0025] The synthetic method of N,N-dimethyltrifluoromethanesulfonamide, its synthetic steps are as follows

[0026] Take 19.16g (0.17mol) of 40wt% dimethylamine aqueous solution and add it to the autoclave, cool down to 0°C, slowly add 15.2g (0.1mol) trifluoromethanesulfonyl fluoride dropwise, after the dropwise addition, add 7.08g (0.07mol) triethylamine, then increase the pressure to 0.1MPa, maintain 0.1MPa and raise the temperature to 15°C for amidation reaction for 22h, after the amidation reaction is completed, concentrate, and then use ether as the eluent to go through column chromatography After purification, the eluate was collected, concentrated, and concentrated under reduced pressure to obtain 15.64 g of N,N-dimethyltrifluoromethanesulfonamide, with a yield of 88.29% and a purity of 99.6%.

Embodiment 3

[0028] The synthetic method of N,N-dimethyltrifluoromethanesulfonamide, its synthetic steps are as follows:

[0029] Take 18.03g (0.16mol) of 40wt% dimethylamine aqueous solution and add it to the autoclave, cool down to 3°C, slowly add 15.2g (0.1mol) trifluoromethanesulfonyl fluoride dropwise, after the dropwise addition, add 6.07g (0.06mol) triethylamine, then increase the pressure to 0.3MPa, maintain 0.3MPa and raise the temperature to 10°C for amidation reaction for 20h, after the amidation reaction is completed, concentrate, and then use ether as the eluent to go through column chromatography After purification, the eluate was collected, concentrated, and concentrated under reduced pressure to obtain 15.73 g of N,N-dimethyltrifluoromethanesulfonamide, with a yield of 88.79% and a purity of 99.6%.

technical field

[0001] The invention relates to the technical field of battery electrolyte additives, in particular to a synthesis method of N,N-dimethyltrifluoromethanesulfonamide. Background technique

[0002] Lithium-ion batteries are currently the most common electrical energy storage devices. Compared with traditional batteries, they have higher storage capacity and more stable performance. The key factors affecting the performance of lithium-ion batteries lie in the performance of organic electrolytes. In battery production, an electrolyte additive containing N,N-dimethyltrifluoromethanesulfonamide is added to the electrolyte to increase the concentration of hydrogen ions in the electrolyte and reduce the loss in the process of electric energy conversion.

[0003] In the prior art, the preparation process of N,N-dimethyltrifluoromethanesulfonamide mainly generates N,N-dimethyltrifluoromethanesulfonamide through the reaction of trifluoromethanesulfonamide and methyl hal...

Examples

Embodiment 1

[0021] The synthetic method of N,N-dimethyltrifluoromethanesulfonamide, its synthetic steps are as follows:

[0022] Take 16.91g (0.15mol) of 40wt% dimethylamine aqueous solution and add it to the autoclave, cool down to 5°C, slowly add 15.2g (0.1mol) trifluoromethanesulfonyl fluoride dropwise, after the dropwise addition, add 8.1g (0.08mol) triethylamine, then increase the pressure to 0.5MPa, maintain 0.5MPa and raise the temperature to 20°C for amidation reaction for 20h, after the amidation reaction is completed, concentrate, and then use ether as the eluent to go through column chromatography Purify, collect, concentrate the eluent, and concentrate under reduced pressure to obtain 15.89 g of N,N-dimethyltrifluoromethanesulfonamide with a yield of 89.70% and a purity of 99.5%. The specific chemical reaction formula is as follows:

[0023]

Embodiment 2

[0025] The synthetic method of N,N-dimethyltrifluoromethanesulfonamide, its synthetic steps are as follows

[0026] Take 19.16g (0.17mol) of 40wt% dimethylamine aqueous solution and add it to the autoclave, cool down to 0°C, slowly add 15.2g (0.1mol) trifluoromethanesulfonyl fluoride dropwise, after the dropwise addition, add 7.08g (0.07mol) triethylamine, then increase the pressure to 0.1MPa, maintain 0.1MPa and raise the temperature to 15°C for amidation reaction for 22h, after the amidation reaction is completed, concentrate, and then use ether as the eluent to go through column chromatography After purification, the eluate was collected, concentrated, and concentrated under reduced pressure to obtain 15.64 g of N,N-dimethyltrifluoromethanesulfonamide, with a yield of 88.29% and a purity of 99.6%.

Embodiment 3

[0028] The synthetic method of N,N-dimethyltrifluoromethanesulfonamide, its synthetic steps are as follows:

[0029] Take 18.03g (0.16mol) of 40wt% dimethylamine aqueous solution and add it to the autoclave, cool down to 3°C, slowly add 15.2g (0.1mol) trifluoromethanesulfonyl fluoride dropwise, after the dropwise addition, add 6.07g (0.06mol) triethylamine, then increase the pressure to 0.3MPa, maintain 0.3MPa and raise the temperature to 10°C for amidation reaction for 20h, after the amidation reaction is completed, concentrate, and then use ether as the eluent to go through column chromatography After purification, the eluate was collected, concentrated, and concentrated under reduced pressure to obtain 15.73 g of N,N-dimethyltrifluoromethanesulfonamide, with a yield of 88.79% and a purity of 99.6%.

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